HRID46448

反应详情

EQUATION

反应方程式

HRID 46448 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 10 g of [o-(3-chloro-o-toluidino)-phenyl]-acetic acid (M.P. 124°-125°) in 100 ml of ether are slowly added dropwise 100 ml of 2% ethereal diazomethane solution. The solution is allowed to stand for 2 hours at room temperature, and then concentrated to dryness at 40° under 11 Torr. The residue is dissolved in 100 ml of ether. The ether solution is extracted with 40 ml of 2 N sodium hydrogen carbonate solution and water, dried over sodium sulphate, and concentrated at 40° under 11 Torr. The residue is crystallised from benzine. The obtained [o-(3-chloro-o-toluidino)-phenyl]-acetic acid methyl ester melts at 47°-48°.

WORKUP

后处理

  1. concentrationconcentrated to dryness at 40° under 11 Torr
  2. dissolutionThe residue is dissolved in 100 ml of ether
  3. extractionThe ether solution is extracted with 40 ml of 2 N sodium hydrogen carbonate solution and water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated at 40° under 11 Torr
  6. customThe residue is crystallised from benzine