HRID1389519

反应详情

EQUATION

反应方程式

HRID 1389519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.8 g. of 5-bromo-6-nitroindan, 4.5 g. of potassium tert.-butylate, 4.4 g. of 2-pyridinethiol are heated in 50 ml. of absolute dimethylformamide for 3 hours under nitrogen to 80°. The mixture is concentrated under vacuum; the residue is combined with ethyl acetate and extracted four times with water. The ethyl acetate phase is concentrated, and the residue is purified on a silica gel column (system: cyclohexane/ethyl acetate 4:1). After crystallization from ethanol, 3.3 g. of 5-nitro-6-(2-pyridylthio)indan is obtained, m.p. 74°.

WORKUP

后处理

  1. concentrationThe mixture is concentrated under vacuum
  2. extractionextracted four times with water
  3. concentrationThe ethyl acetate phase is concentrated
  4. customthe residue is purified on a silica gel column (system: cyclohexane/ethyl acetate 4:1)
  5. customAfter crystallization from ethanol, 3.3 g