HRID235085

反应详情

EQUATION

反应方程式

HRID 235085 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 5.0 g (39.02 mmol) of thiophene-2-carboxylic acid (Aldrich Chemical Co.) in 100 mL of methylene chloride stirred at 0° C. was added 11 g (82.5 mmol) of AICl3 and 5.8 g (43.0 mmol) of t-butyl bromide. The solution was stirred at room temperature for 18 hours then poured into 100 mL of ice water, and the mixture was extracted with ether. The extracts were washed with brine and dried over MgSO4, then concentrated to give 3.33 g of the title product. MS (M+H)+ : 202. NMR (CDCl3) δ:1.42 (s, 9H), 6.89 (d, 1H, J=4 Hz), 7.72 (d, 1H, J=4 Hz).

WORKUP

后处理

  1. extractionthe mixture was extracted with ether
  2. washThe extracts were washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated