HRID583238

反应详情

EQUATION

反应方程式

HRID 583238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of 7-nitro-3,4-dihydroisoquinoline (10.0 g, 56.1 mmol) and malonic acid (11.7 g, 112 mmol) in acetic acid (55 ml) was heated at 120° C. for 0.5 h. Upon cooling, the solvent was concentrated to give a red oil which was taken up in aqueous ethanol (50 ml of 75%). After crystallization had occurred, the solvent was cooled to 0° C. and the product collected. The title compound was isolated as a tan solid (10.9 g, 81%), m.p. 264-5° C. (dec.).

WORKUP

后处理

  1. temperatureUpon cooling
  2. concentrationthe solvent was concentrated
  3. customto give a red oil which
  4. customAfter crystallization
  5. temperaturethe solvent was cooled to 0° C.
  6. customthe product collected