HRID1266145

反应详情

EQUATION

反应方程式

HRID 1266145 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-cyano-2-ethoxycarbonyl-4-nitroindan (21 g, 81 mmol), acetic acid (290 mL), hydrochloric acid (37%, 130 mL) and water (140 mL) was stirred under reflux temperature over night. The acid was evaporated in vacuo and the residue was made alkaline with a 2 M sodium hydroxide solution. The mixture was stirred at room temperature, insoluble matter was filtered and the filtrate was acidified with hydrochloric acid. The obtained precipitate was filtered and washed with water to afford 18 gram of the crude acid: mp ˜140° C.; EIMS (70 eV) m/z (relative intensity) 207 (40, M+).

WORKUP

后处理

  1. temperatureunder reflux temperature over night
  2. customThe acid was evaporated in vacuo
  3. stirringThe mixture was stirred at room temperature
  4. filtrationinsoluble matter was filtered
  5. filtrationThe obtained precipitate was filtered
  6. washwashed with water