HRID589665

反应详情

EQUATION

反应方程式

HRID 589665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-methyl-benzothiophene (900 mg, 6.1 mmol), Ac2O (1.75 mL, 18.5 mmol) and conc. H2SO4 (350 μL, 6.2 mmol) in EtOAc (5 mL) was stirred at room temperature for 3 h. The reaction mixture was diluted with EtOAc. The organic phase was washed with water and brine and then dried. Upon evaporation of some of the solvent the product precipitated. Et2O was added, and the precipitate was collected giving 193 mg of 3-methylbenzothiophene-2-sulfonic acid (14%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.48 (s, 3 H) 7.33-7.41 (m, 2 H) 7.69-7.75 (m, 1 H) 7.83-7.88 (m, 1 H).

WORKUP

后处理

  1. washThe organic phase was washed with water and brine
  2. customdried
  3. customUpon evaporation of some of the solvent the product
  4. customprecipitated
  5. additionEt2O was added
  6. customthe precipitate was collected