HRID1244912

反应详情

EQUATION

反应方程式

HRID 1244912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The operation is carried out as in Stage 2 of Example 5 starting from 160 mg of the product obtained in Stage 1 of Example 5, 3 ml of butanol and using 0.055 ml of aniline in place of the benzylamine and the reaction medium is taken to a temperature of approximately 80 to 85° C. for 20 hours, left to return to ambient temperature, diluted with 5 ml of isopropanol, placed for approximately one hour at a temperature of approximately 0° C., followed by separating, washing with 5 ml of isopropanol and drying under vacuum to a temperature of approximately 50° C. After purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 90/10, 173 mg of expected product is thus obtained in the form of white crystals.

WORKUP

后处理

  1. waitleft
  2. customto return to ambient temperature
  3. waitplaced for approximately one hour at a temperature of approximately 0° C.
  4. customby separating
  5. washwashing with 5 ml of isopropanol
  6. customdrying under vacuum to a temperature of approximately 50° C
  7. customAfter purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 90/10, 173 mg of expected product
  8. customis thus obtained in the form of white crystals