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
The 2-(2,4-dichlorophenyl)-1-(2-chlorothiazol-5-yl)propan-2-ol (6.4 g) obtained in Example 1 was dissolved in acetic acid (80 ml) and the mixture brought to reflux whereupon zinc dust (3.5 g) was added and the mixture was stirred under reflux for a further 2 hours and then cooled. Dilute ammonium hydroxide solution was added until the reaction mixture was basic and the mixture was then extracted into ethyl acetate (2×200 ml). The combined extract was washed with brine (50 ml), dried and then concentrated under reduced pressure. Flash chromatography of the residue on a silica gel column using petroleum ether-ethyl acetate as eluant gave 2-(2,4-dichlorophenyl)-1-(thiazol-5-yl)propan-2-ol (3.2 g) as a white solid, m.pt. 164° C.
WORKUP
后处理
- additionwas added
- temperatureunder reflux for a further 2 hours
- temperaturecooled
- extractionthe mixture was then extracted into ethyl acetate (2×200 ml)
- extractionThe combined extract
- washwas washed with brine (50 ml)
- customdried
- concentrationconcentrated under reduced pressure