Methyl chloroformate → HCID 56973781、化合物

反応式

[CH3:1][O:2][C:3](Cl)=[O:4].C(N(CC)CC)C.[C:13]([NH:17][C:18](=[O:27])[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([NH2:26])[CH:21]=1)([CH3:16])([CH3:15])[CH3:14]>CC(C)=O>[C:13]([NH:17][C:18](=[O:27])[CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([NH:26][C:3]([O:2][CH3:1])=[O:4])[CH:21]=1)([CH3:16])([CH3:14])[CH3:15]

参加物

反応条件

温度: 17.5 °C

実験手順

10.45 g (0.1 mol) of chloroformic acid methyl ester, followed by 10.1 g (0.1 mol) of triethylamine, were added dropwise to a solution of 20.6 g (0.1 mol) of 3-amino-phenylacetic acid tert.-butylamide in 200 ml of acetone whilst cooling at 15 to 20° C. The mixture was stirred for a further 2 hours at room temperature, the triethylamine hydrochloride which had precipitated was filtered off and the filtrate was concentrated by evaporation under reduced pressure. The residue which hereupon remained was stirred with very dilute hydrochloric acid, filtered off, dried and recrystallized from a little carbon tetrachloride. 22 g (83.5% of theory) of 3-methoxycarbonylamino-phenylacetic acid tert.-butylamide of melting point 123°-124° C were obtained.