HRID545477

反应详情

EQUATION

反应方程式

HRID 545477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-trityloxycarbamoyl -benzo[b]thiophene-5-carboxylic acid methyl ester (4.439 g, 8.99 mmol) in THF (50 mL) and 2M aqueous NaOH (50 mL) was allowed to stir at rt for six days. After removal of THF, the aqueous phase was acidified with HOAc/H2O (1:1) to pH≈4. The solid formed was filtered, collected and dried to give 2-trityloxycarbamoyl-benzo[b]thiophene-5-carboxylic acid as a white solid. 1H NMR (DMSO-d6, 200 MHz) δ 11.33 (brs, 1H), 8.47 (s, 1H), 8.10-7.80 (m, 3H), 7.56-7.14 (m, 15H). MS (EI): cal'd 243.1 (M-benzothiophene moiety+H+,) exp 243.1 (M-benzothiophene moiety+H+).

WORKUP

后处理

  1. customAfter removal of THF
  2. customThe solid formed
  3. filtrationwas filtered
  4. customcollected
  5. customdried