[(1S)-1-甲基-2-(甲基氨基)乙基]氨基甲酸叔丁酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 6.00 ml methylamine solution (2 M in tetrahydrofuran) are added to 1.73 g tert.butyl ((S)-1-methyl-2-oxoethyl)-carbamate in 20 ml benzene with stirring at ambient temperature. Then 2.50 g anhydrous sodium sulphate are added and the reaction mixture is stirred overnight at ambient temperature. The sodium sulphate is suction filtered and washed again with benzene. The filtrate is evaporated down, taken up in 20 ml of methanol and combined with 397 mg sodium cyanoborohydride with stirring at ambient temperature. After 2.5 hours the reaction mixture is acidified by dropwise addition of approx. 20 ml 2 N citric acid and extracted with tert.-butylmethylether. The aqueous phase is made alkaline with 10 M sodium hydroxide solution and extracted with a methylene chloride/methanol mixture. The combined organic phases are dried over magnesium sulphate and evaporated down. the reaction mixture is stirred overnight at ambient temperature filtered washed again with benzene The filtrate is evaporated down with stirring at ambient temperature After 2.5 hours the reaction mixture is acidified by dropwise addition of approx. 20 ml 2 N citric acid extracted with tert.-butylmethylether extracted with a methylene chloride/methanol mixture The combined organic phases are dried over magnesium sulphate evaporated down