HRID261511

反应详情

EQUATION

反应方程式

HRID 261511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe reaction mixture was filtered
  2. washwashed with anhydrous acetone
  3. concentrationThe filtrate was concentrated under 10 mmHg
  4. temperaturewithout heating
  5. customThe residue was recrystallized from ethanol