Downstream synthetic route of 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

1632-76-4, 3-Methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

a 3-Chloromethylpyridazine Trichloroisocyanuric acid (1.04 g, 4.46 mmol) was added to a boiling solution of 3-methylpyridazine (1.00 g, 10.6 mmol) in chloroform (30 ml) under nitrogen and the mixture heated at reflux overnight. The mixture was cooled to room temperature, diluted with dichloromethane and filtered through a pad of celite. The filtrate was washed with 1N sodium hydroxide solution (2*100 ml) and brine (*2), dried (MgSO4) and evaporated in vacuo to give 3-chloromethylpyridazine., 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

Reference£º
Patent; Merck Sharp & Dohme Limited; US6200975; (2001); B1;,
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Analyzing the synthesis route of 1632-76-4

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1632-76-4,3-Methylpyridazine,as a common compound, the synthetic route is as follows.

1632-76-4, General procedure: K2[M'(CN)4].H2O was prepared by mixing the stoichiometric amounts of nickel(II) chloride hexahydrate (1 mmol, 0.238 g) or palladium(II) chloride (1 mmol, 0.177 g) or platinum(II) chloride(1 mmol, 0.266 g) in water (10 mL) solutions with potassiumcyanide (4 mmol, 0.260 g) in water (10 mL) solutions. These solutions were filtered and allowed to evaporate at room temperature in order to crystallize. The K2[M'(CN)4]H2O (1 mmol) complexes(M’ , 0.259 g for Ni(II), 0.306 g for Pd(II), 0.395 g for Pt(II)) were dissolved in water (50 mL). To these solutions, 1 mmol of zinc(II) chloride or 1 mmol of cadmium(II) chloride hemi(pentahydrate)dissolved in water (10 mL) were added with continuous stirring approximately for 4h at 50¡ãC in a temperature-controlled bath.The M[M'(CN)4]H2O compounds obtained were filtered and dried in air. The complexes were prepared by mixing together with the50 mL of water solution of 1 mmol of Zn[Ni(CN)4]H2O = 0.246 g,Zn[Pd(CN)4]H2O = 0.293 g or Zn[Pt(CN)4]H2O = 0.382 g, separately.To M[M'(CN)4]H2O solutions, 3-mpdz (2 mmol, 0.188 g) dissolved in ethanol (10 mL) was added with continuous stirring and after afew minutes ammonia (5 mL, 28percent) was added a few drops to resulting solution with continuous stirring approximately for 5h at 60¡ãCin a temperature-controlled bath and then filtered. The resulting clear solutions were kept for crystallization at room temperature. In the meantime, the ammonia was moved away from the solutions itself. Within about a week bright crystals were obtained. The procedure for the syntheses of cadmium complexes was similar to that used for zinc complexes, except that the Zn[M'(CN)4]H2Owas used instead of Cd[M'(CN)4]H2O [Cd[Ni(CN)4]H2O = 0.246 g,Cd[Pd(CN)4]H2O = 0.340 g or Cd[Pt(CN)4]H2O = 0.429 g]. The C, H,N analyses were carried out for the complexes and were found tofit the proposed formulae well.

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Goer, Kansu; Kuerkcueo?lu, Guene? Sueheyla; Ye?ilel, Okan Zafer; Bueyuekguengoer, Orhan; Inorganica Chimica Acta; vol. 414; (2014); p. 15 – 20;,
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Downstream synthetic route of 1632-76-4

1632-76-4, As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

1632-76-4, 3-Methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(i) 1-(2,4-Difluorophenyl)-2-(pyridazin-3-yl)ethanone Treatment of 3-methylpyridazine (4.70 g) with lithium diisopropylamide (0.05 mole) in dry tetrahydrofuran followed by methyl 2,4-difluorobenzoate (8.60 g) according to the method of Example 11(i) gave the title compound, (3.40 g), m.p. 115.5¡ã-117.5¡ã (from ether).

1632-76-4, As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

Reference£º
Patent; Pfizer Inc.; US5116844; (1992); A;,
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Brief introduction of 1632-76-4

1632-76-4, The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

1632-76-4, 3-Methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step A: 6-methylpyridazine-3-carbonitrile (2)To a stirring solution of 3-methylpyridazine (1.1 g, 11.80 mmol) in dichloromethane (20 mL) was added AICI3(0.05 g) followed by trimethylsilylcyanide (2.1 g, 21.1 mmol). After 20 min, a solution of p-toluenesulfonyl chloride (3.8 g, 20.1 mmol) in dichloromethane (5 mL) was added slowly and the solution was stirred for 16 h. The solvent was removed in vacuo and ethanol (10 ml) was added and stirred for 15 min, then filtered to give a white solid. The solid was dissolved in THF (200 mL) and DBU (1.6 mL, 10.5 mmol) was added. After 1 h, the solvent was removed in vacuo and the residue was partitioned between hexane and saturated aqueous NH4C1. The aqueous phase was basified with solid a2C03, and then extracted with EtOAc (100ml*2). The combined ethyl acetate phases was dried over MgS04, filtered and concentrated to give compound 2 as a white solid.

1632-76-4, The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; MERCK SHARP & DOHME CORP.; KUDUK, Scott, D.; MCCOMAS, Casey, C.; REGER, Thoma, S.; QI, Changhe; WO2014/150114; (2014); A1;,
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Downstream synthetic route of 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

1632-76-4, 3-Methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 19; S-CS^-Dimethyl-lH-indol-l-yO-N’-CS-methoxy^-Cpyridazin-S- ylmethoxy)benzylidene)propanehydrazide; [0529] (a) 3-(Chloromethyl)pyridazine: To a stirred solution of 3- methylpyridazine (0.29 niL, 3.19 mmol) in CHCl3 (6 niL) at 60 0C was added trichloroisocyanuric acid (296 mg, 1.28 mmol) in several portions. The reaction mixture was heated for 2 hours and then absorbed directly onto silica gel. Purification on silica gel using EtOAc -hexane (0 to 80%) provided the product as a reddish oil (160 mg)., 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

Reference£º
Patent; STEIN, Philip; DAINES, Robert; SPROUS, Dennis; O’GRADY, Harold; WO2010/132615; (2010); A1;,
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Analyzing the synthesis route of 1632-76-4

1632-76-4, The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1632-76-4,3-Methylpyridazine,as a common compound, the synthetic route is as follows.

To a solution of 3-methylpyridazine (4.60 g, 48.9 mmol) in acetic acid (30.0 mL) was added H202 (29.4 g,259 mmol, 29.4 mL, 30percent (w/w) in water). The mixture was heated at 120 00 for 6 h. The mixture wasallowed to cool to rt and poured in aqueous saturated NaHCO3 (500 mL) and extracted with DCM (5x 50 mL). The combined organic layer was dried over Na2SO4 and concentrated in vacuo to afford 6-methyl- pyridazine 1-oxide (2.22 g, 20.2 mmol, 41percent). LCMS: cal for [M+H} = 111.05, fd 111.2. 1H NMR shows a 1:1 mixture of both possible N-oxides.

1632-76-4, The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GRUeNENTHAL GMBH; NARDI, Antonio; RATCLIFFE, Paul; CRAAN, Tobias; HERTRAMPF, Thorsten; LESCH, Bernhard; STEINHAGEN, Henning; (70 pag.)WO2015/161924; (2015); A1;,
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Brief introduction of 1632-76-4

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

1632-76-4, 3-Methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A) Preparation of 3-methyl-6-cyanopyridazine To a stirring solution of 3-methylpyridazine (11 g, 118 mmol) in dichloromethane (200 mL) was added AlCl3 (0.05 g) followed by trimethylsilylcyanide (21 g, 211 mmol). After 20 min, a solution of p-toluenesulfonyl chloride (38 g, 201 mmol) in dichloromethane (50 mL) was added via addition funnel and the solution continued to stir overnight. The next morning, the solvent was removed in vacuo and the residue was suspended in ethanol with stirring for 15 min and then filtered to give a white solid. The solid was dissolved in tetrahydrofuran (200 mL) and to this stirring solution was added 1,8-diazabicyclo[5.4.0]undec-7-ene (16 mL, 105 mmol). After 1 h, the solvent was removed in vacuo and the residue was partitioned between hexanes and saturated aqueous NH4 Cl. The phases were separated and the aqueous phase was basified with solid Na2 CO3, then extracted three times with ethyl acetate. The combined ethyl acetate phases were dried (MgSO4), filtered and concentrated in vacuo to give 9 g (64percent) of white solid., 1632-76-4

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Eli Lilly and Company; US5710130; (1998); A;,
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New learning discoveries about 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1632-76-4,3-Methylpyridazine,as a common compound, the synthetic route is as follows.

EXAMPLE 69 STR99 Preparation of 3-methyl-6-cyanopyridazine To a stirring solution of 3-methylpyridazine (11 g, 118 mmol) in dichloromethane (200 mL) was added AlCl3 (0.05 g) followed by trimethylsilylcyanide (21 g, 211 mmol). After 20 min, a solution of p-toluenesulfonyl chloride (38 g, 201 mmol) in dichloromethane (50 mL) was added via addition funnel and the solution continued to stir overnight. The next morning, the solvent was removed in vacuo and the residue was suspended in ethanol with stirring for 15 min and then filtered to give a white solid. The solid was dissolved in tetrahydrofuran (200 mL) and to this stirring solution was added 1,8-diazabicyclo[5.4.0]undec-7-ene (16 mL, 105 mmol). After 1 h, the solvent was removed in vacuo and the residue was partitioned between hexanes and saturated aqueous NH4 Cl. The phases were separated and the aqueous phase was basified with solid Na2 CO3, then extracted three times with ethyl acetate. The combined ethyl acetate phases were dried (MgSO4), filtered and concentrated in vacuo to give 9 g (64percent) of white solid., 1632-76-4

As the paragraph descriping shows that 1632-76-4 is playing an increasingly important role.

Reference£º
Patent; Eli Lilly and Company; US5707966; (1998); A;,
Pyridazine – Wikipedia
Pyridazine | C4H4N2 – PubChem

 

Analyzing the synthesis route of 1632-76-4

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1632-76-4,3-Methylpyridazine,as a common compound, the synthetic route is as follows.,1632-76-4

General procedure: Methyldiazine derivative (1mmol) and compound 3 (1.1equiv per methyl group) were dissolved in THF (20mL). tBuOK (1.5equiv per methyl group) was slowly added at room temperature. The solution, which immediately turned brown, was then refluxed overnight. After cooling, water was added, THF was evaporated and the mixture extracted with CH2Cl2, dried over MgSO4 and the solvent removed under vacuum.

The synthetic route of 1632-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Achelle, Sylvain; Kahlal, Samia; Saillard, Jean-Yves; Cabon, Nolwenn; Caro, Bertrand; Robin-Le Guen, Franc?oise; Tetrahedron; vol. 70; 17; (2014); p. 2804 – 2815;,
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Some tips on 1632-76-4

1632-76-4 3-Methylpyridazine 74208, apyridazine compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1632-76-4,3-Methylpyridazine,as a common compound, the synthetic route is as follows.

A solution of 3-Methylpyridazine 15 (5.0 g, 53.0 mmol) in THF (10 mL) was added to potassium tert-butoxide (8.9 g, 80.0 mmol) in THF (50 mL) at 0 C. After stirring at room temperature for 1.5 hours, tert-butyl nitrite (12.6 mL, 106 mmol) in THF (10 mL) was added to the reaction mixture at 0 C. After stirring at room temperature for 19 hours, the solvent was removed in vacuo and the residue was added to 4 M HCl solution (20 mL). The resulting mixture was concentrated in vacuo and filtered a colorless powder of aldoxime 16a (1.8 g). The residue was extracted with ethylacetate (50 mL 3). The organic layer was dried over MgSO4. The solvent was removed in vacuo, then triturated with n-hexane to yield aldoxime 16a (2.8 g). The combined aldoxime 16a (4.6 g, 71%) was E, Z mixture of isomer. N-Chlorosuccimide (4.0g, 30 mmol) was added to a suspension of 16a (3.7 g, 30 mmol), ethynyl tri-n-butylstannane (9.3 g, 20 mmol), NaHCO3 (6.3 g, 75 mmol), ethyacetate (100 mL) and distilled water (5 mL). After stirring at room temperature for 16 hours, distilled water (5 mL) was added to the reaction mixture. After stirring at room temperature for 4 hours, the reaction mixture was washed with saturated NaHCO3 (100 mL), and the aqueous layer was extracted with ethylacetate (100 mL). The combined organic layer was dried over MgSO4. The solvent was removed in vacuo and the residue was used in the next reaction without further purification. The crude 17a was dissolved in THF (100 mL). Iodine (3.2 g, 25.2 mmol) was added to the solution at room temperature. After stirring at room temperature for 35 minutes, the reaction mixture was diluted with 6% sodium thiosulfate solution (100 mL) and extracted with ethylacetate (100 ml). The organic layer was washed with brine and dried over MgSO4. The solvent was removed in vacuo and the residue was recrystallized from n-hexane to yield compound 14a (2.9 g, 35% for two steps) as a brown powder

1632-76-4 3-Methylpyridazine 74208, apyridazine compound, is more and more widely used in various.

Reference£º
Article; Sugimoto, Tomohiro; Shimazaki, Yoichi; Manaka, Akira; Tanikawa, Tetsuya; Suzuki, Keiko; Nanaumi, Kayoko; Kaneda, Yoshie; Yamasaki, Yukiko; Sugiyama, Hiroyuki; Bioorganic and Medicinal Chemistry Letters; vol. 22; 17; (2012); p. 5739 – 5743;,
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