HRID1156174

反应详情

EQUATION

反应方程式

HRID 1156174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.76 g. of 8-chlorodibenzothiophene-3-acetic acid, 3.04 g. of potassium carbonate, 1.73 g. of dimethylaminoethyl chloride hydrochloride, and 250 ml. of dimethylformamide was stirred and heated at 120° for 4 hours. The solvent was removed in vacuo on the steam bath, and 75 ml. of water added to the residue. The oil was extracted with ethyl acetate and the crude product precipitated as the hydrochloride by the addition of hydrogen chloride. On crystallization from acetone, 1.5 g. of 8-chlorodibenzothiophene-3-acetic acid 2-dimethylaminoethyl ester hydrochloride, m.p. 179°-181°, was obtained.

WORKUP

后处理

  1. additionA mixture of 2.76 g
  2. temperatureheated at 120° for 4 hours
  3. customThe solvent was removed in vacuo on the steam bath, and 75 ml
  4. additionof water added to the residue
  5. extractionThe oil was extracted with ethyl acetate
  6. customthe crude product precipitated as the hydrochloride by the addition of hydrogen chloride
  7. customOn crystallization from acetone, 1.5 g