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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of 6.5 g of methyl 2-(2,6-dichloroanilino)phenylglyoxylate in 130 ml of ethanol was added 0.5 g of sodium borohydride while cooling at -15° to -20° C., and the mixture was stirred at 0° C. for 2 hours and then at room temperature for further 1 hour. Thereafter, the reaction mixture was mixed with diluted hydrochloric acid for decomposition, diluted with 500 ml of water and extracted with ether. The ether extract was washed with water, dried over anhydrous sodium sulfate and then concentrated without heating. The resulting residue was recrystallized from ethanol to give 6.2 g of methyl 2-(2,6-dichloroanilino)phenylglycolate. m.p. 123°-124° C. Yield: 95% of theoretical amount
WORKUP
后处理
- temperaturewhile cooling at -15° to -20° C.
- waitat room temperature for further 1 hour
- extractionextracted with ether
- extractionThe ether extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- temperaturewithout heating
- customThe resulting residue was recrystallized from ethanol