HRID510100

反应详情

EQUATION

反应方程式

HRID 510100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

146 mg (0.435 mmol) of the compound from example 43A were initially charged in ethanol (8 ml), then 69 mg (0.48 mmol) of ethyl 3-methyl-2-oxobutanoate were added and the reaction mixture was heated to reflux overnight. Thereafter, a catalytic amount of conc. sulfuric acid was added and the mixture was again heated to reflux overnight. Subsequently, the mixture was cooled to RT, and the solid formed was filtered off, washed with methanol and dried under high vacuum. This gave 26 mg (14% of theory) of the title compound in solid form.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux overnight
  3. temperaturethe mixture was again heated
  4. temperatureto reflux overnight
  5. customthe solid formed
  6. filtrationwas filtered off
  7. washwashed with methanol
  8. customdried under high vacuum