HRID2391952

反应详情

EQUATION

反应方程式

HRID 2391952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of bromine (634 uL, 12.3 mmol) in AcOH (2.5 mL) was added dropwise to 5-chloro-2-thiophenecarboxylic acid (2 g, 12.3 mmol) and FeCl3 (399 mg, 2.50 mmol) in AcOH (25 mL) at 25° C. The reaction mixture was warmed to reflux where additional bromine (634 uL, 12.3 mmol) and FeCl3 (399 mg, 2.50 mmol) were added. After 7 d, the solution was poured onto ice and the precipitate was filtered and washed with water affording the title compound (3 g, quant.) as a yellow powder: LCMS (ES) m/z 242 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed
  2. additionwere added
  3. additionthe solution was poured onto ice
  4. filtrationthe precipitate was filtered
  5. washwashed with water affording the title compound (3 g, quant.) as a yellow powder