HRID477542

反应详情

EQUATION

反应方程式

HRID 477542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a sodium methoxide solution, prepared from 1.4 g of sodium and 50 ml of methanol, was added all at once the product obtained in Step 1 of Example 43 (4.6 g under ice cooling. The mixture was refluxed for one hour, the solution was concentrated under reduced pressure, and the remaining yellow oil was dissolved in 50 ml water. The pH was adjusted to 1.0 with 1N hydrochloric acid, and the formed crystals were collected by filtration and washed with 30 ml ethanol, giving 1.7 g of the objective compound as faint yellow crystals.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for one hour
  2. concentrationthe solution was concentrated under reduced pressure
  3. dissolutionthe remaining yellow oil was dissolved in 50 ml water
  4. filtrationthe formed crystals were collected by filtration
  5. washwashed with 30 ml ethanol