HRID1166210

反应详情

EQUATION

反应方程式

HRID 1166210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(3,5-Dibromothiophen-2-yl)-oxo-acetic acid ethyl ester (513 mg, 1.50 mmol) was dissolved in 25 ml acetone and treated with 15 ml 8 N HCl at reflux for a total of 4 hours. The reaction mixture was concentrated in vacuo, poured into 50 ml water, and extracted into 100 ml of dichloromethane. The organic layer was dried over Na2SO4 and concentrated in vacuo to yield (3,5-dibromothiophen-2-yl)-oxo-acetic acid (467 mg, 99%). MS (M+H)+: 314.84; 1H NMR (300 MHz, DMSO-d6) δ7.64 (1H, s).

WORKUP

后处理

  1. temperatureat reflux for a total of 4 hours
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additionpoured into 50 ml water
  4. extractionextracted into 100 ml of dichloromethane
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated in vacuo