HRID1672722

反应详情

EQUATION

反应方程式

HRID 1672722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

Add trans-4-aminocyclohexanol (230 g, 2.0 mol) to γ-butyrolactone (140 mL, 1.82 mol) in a 1 L round-bottom flask equipped with large magnetic stirrer, thermometer and condenser/nitrogen bubbler. Heat the mixture at 190° C. for 68 hours. Cool to ambient temperature and mix with water (1 L). Extract into dichloromethane (10×1.5 L). Dry the extracts over magnesium sulfate, filter and evaporate to a brown solid. Triturate with diethyl ether to afford 144.7 g (43%) of the title compound: MS (m/z): 184 (M+1).

WORKUP

后处理

  1. customequipped with large magnetic stirrer
  2. temperatureCool to ambient temperature
  3. extractionExtract into dichloromethane (10×1.5 L)
  4. dry with materialDry the extracts over magnesium sulfate
  5. filtrationfilter
  6. customevaporate to a brown solid
  7. customTriturate with diethyl ether