HRID2116685

反应详情

EQUATION

反应方程式

HRID 2116685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 0.64 g (15 mmol) lithium hydroxide hydrate in 100 mL water was added to a suspension of 6.0 g (10.31 mmol) ethyl (R)-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-{[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzdiazepin-3-yl)-piperidine-1-carbonyl]-amino}-propionate in 50 mL THF. In each case 100 mL water and THF were again added to this suspension, and a solution formed after 5 min. This was stirred for 1 hour at RT, the THF was eliminated i.vac., the remainder was diluted with 100 mL water and 1 M aqueous hydrochloric acid solution was added dropwise while cooling with ice until an acid reaction was obtained. The precipitated substance was filtered, washed with water and dried in the air.

WORKUP

后处理

  1. customa solution formed after 5 min
  2. additionwas added dropwise
  3. temperaturewhile cooling with ice until an acid reaction
  4. customwas obtained
  5. filtrationThe precipitated substance was filtered
  6. washwashed with water
  7. customdried in the air