HRID2085224
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Salicylaldehyde (293 g) and Υ-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
- temperaturethe solution was cooled to not more than 3° C. in an ice-salt bath
- customrose to 24° C
- stirringthe mixture was stirred for 45 min
- temperatureunder heating at 60-65° C
- temperatureThe reaction mixture was cooled again in an ice-bath
- filtrationThe obtained white suspension was filtrated
- washwashed with water
- customdried