HRID460655

反应详情

EQUATION

反应方程式

HRID 460655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Salicylaldehyde (293 g) and γ-butyrolactone (413 g) were dissolved in toluene (2.4 L) and the solution was cooled to not more than 3° C. in an ice-salt bath. Thereto was added sodium methoxide (324 g) over 20 min. The temperature of the reaction mixture rose to 24° C. After stirring at room temperature for 3 hr, the mixture was stirred for 45 min under heating at 60–65° C. The reaction mixture was cooled again in an ice-bath and 10% sulfuric acid (2.51 ml) was added dropwise. The obtained white suspension was filtrated, washed with water and dried to give the title compound (324 g), melting point 162–164° C.

WORKUP

后处理

  1. temperaturethe solution was cooled to not more than 3° C. in an ice-salt bath
  2. customrose to 24° C
  3. stirringthe mixture was stirred for 45 min
  4. temperatureunder heating at 60–65° C
  5. temperatureThe reaction mixture was cooled again in an ice-bath
  6. filtrationThe obtained white suspension was filtrated
  7. washwashed with water
  8. customdried