HRID66133

反应详情

EQUATION

反应方程式

HRID 66133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Hydroxy-5-oxo-1,3,6-cycloheptatrien-1-ylamino)-2-butenedioic acid diethyl ester (100 g, described in Example 1) is added in portions over 5 minutes to diphenyl ether (1000 ml) at reflux temperature. The solution is refluxed for 25 minutes and cooled to room temperature. Hexane (2000 ml) is added and the crystalline precipitate is collected. The precipitate is crystallized from acetic acid to obtain crystals of the title compound, mp > 300° C. and ν max 3270, 3170, 3100, 1740, 1620 and 1575 cm-1.

WORKUP

后处理

  1. temperatureat reflux temperature
  2. temperatureThe solution is refluxed for 25 minutes
  3. customthe crystalline precipitate is collected
  4. customThe precipitate is crystallized from acetic acid