25808-30-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 25808-30-4 name is 2-(Methylamino)acetonitrile hydrochloride, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
[Example 50] Preparation of 3-methyl-1-(4-methylbenzyl)-4-(4-phenoxyphenyl)iminoimidazolidine-2-one (I-363) To a mixture of 4-methylbenzylamine hydrochloride (10 g, 83 mmol) and N,N-dimethylacetamide (50 mL) was added 1,1′-carbonyldiimidazole (14.05 g, 87 mmol) under ice-cooling. To the mixture was added DBU (18.66 mL, 124 mmol), and the resulting mixture was stirred at 0¡ãC for 30 minutes. To the reaction mixture was added 2-(methylamino)acetonitrile hydrochloride (10.55 g, 99 mmol) under ice-cooling. Further, to the mixture was added DBU (24.88 mL, 165 mmol) under ice-cooling, and the resulting mixture was stirred at room temperature for 45 minutes and stirred at 50¡ãC for additional 90 minutes. To the reaction mixture was added water (500 mL). The mixture was extracted with ethyl acetate (500 mL*2), washed by brine (500 mL), dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resulting residue was purified by silica gel column chromatography (methanol/chloroform) to give 4-imino-3-methyl-1-(4-methylbenzyl)imidazolidine-2-one (9.43 g, Yield:52percent) as yellow solid. 1H-NMR (delta ppm TMS/CDCl3): 2.31 (3H, s), 2.94 (3H, s), 3.93 (2H, s), 4.66 (2H, s), 6.90 (1H, br.s), 7.11 (2H, d, J=8.2 Hz), 7.27 (2H, d, J=8.2 Hz).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(Methylamino)acetonitrile hydrochloride, and friends who are interested can also refer to it.
Reference:
Patent; Shionogi & Co., Ltd.; KAI, Hiroyuki; ENDOH, Takeshi; JIKIHARA, Sae; ASAHI, Kentaro; HORIGUCHI, Tohru; EP2604260; (2013); A1;,
Nitrile – Wikipedia,
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