HRID1060583
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
Hydrazine (18.4 ml, 0.378 moles) was added to a suspension of 3-(3,5-dichloro-pyridin-4-ylmethylen)-6-methoxy-3H-isobenzofuran-1-one (24.4 g, 0.126 moles), obtained as described in example 11, in CH3OH (200 ml), under N2. The mixture was heated under reflux for 1 hour, then kept overnight at room temperature, cooled in ice, and the solid was filtered, washed with very cold CH3OH and dried in oven at 50° C. under vacuum, to give 33.3 g of the title compound (yield: 80%). m.p.: 259-262° C.
WORKUP
后处理
- customobtained
- temperatureThe mixture was heated
- temperatureunder reflux for 1 hour
- temperaturecooled in ice
- filtrationthe solid was filtered
- washwashed with very cold CH3OH
- customdried in oven at 50° C. under vacuum