HRID660904

反应详情

EQUATION

反应方程式

HRID 660904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 3.41 g (12.27 mmol) of the compound from Example 231A in 14 ml methanol/water (7:3) is added dropwise to a solution of 995 mg (12.27 mmol) of potassium isocyanate in 11 ml methanol/water (7:3). This is stirred for 1 hr at RT. The thick suspension is diluted with 7.4 ml water and 39 ml methanol to facilitate stirring, then heated under reflux for 1 hr and then left to stand overnight at RT. After cooling to 0° C., the precipitate is filtered off, washed with ice-cold water and dried overnight in the drying cabinet at 60° C. 2.84 g (76% of theory) of the title compound are obtained.

WORKUP

后处理

  1. stirringto facilitate stirring
  2. temperatureheated
  3. temperatureunder reflux for 1 hr
  4. waitleft
  5. waitto stand overnight at RT
  6. temperatureAfter cooling to 0° C.
  7. filtrationthe precipitate is filtered off
  8. washwashed with ice-cold water
  9. customdried overnight in the drying cabinet at 60° C