HRID261511
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
To a solution of 12.4 g of 2-(2,6-dichloroanilino)-phenylglyoxylic acid in 80 ml of anhydrous acetone were added 6.05 g of anhydrous potassium carbonate and then 7.5 ml of dimethyl sulfate at room temperature, and the mixture was stirred for 1 hour. The reaction mixture was filtered and washed with anhydrous acetone. The filtrate was concentrated under 10 mmHg without heating. The residue was recrystallized from ethanol to give 12.3 g of methyl 2-(2,6-dichloroanilino)phenylglyoxylate as yellow prisms. m.p. 124.5-125.5° C. Yield: 95% of theoretical amount
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- washwashed with anhydrous acetone
- concentrationThe filtrate was concentrated under 10 mmHg
- temperaturewithout heating
- customThe residue was recrystallized from ethanol