HRID551601

反应详情

EQUATION

反应方程式

HRID 551601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
82.5 °C

PROCEDURE

实验过程

N-[-2-(3-amino-4-methoxyphenyl)ethyl]acetamide hydrochloride (19 g) was mixed with 40 mL N,N-dimethylformamide and 18 g of diketene followed by slow addition of 3 mL of triethylamine. The mixture was stirred at 80-85° C. for 30 minutes and then poured into 300 mL of water. The aqueous solution was extracted with chloroform (2×200 mL) and the solvent was removed by rotary evaporation to yield 21.9 g (96.5%) of N-[5-(2-acetylaminoethyl)-2-methoxyphenyl]-3-oxo-butyramide as a light yellow oil. 1HNMR (DMSO-d6) spectrum was consistent with the desired product.

WORKUP

后处理

  1. extractionThe aqueous solution was extracted with chloroform (2×200 mL)
  2. customthe solvent was removed by rotary evaporation