HRID415980
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customequipped with large magnetic stirrer
- temperatureCool to ambient temperature
- extractionExtract into dichloromethane (10×1.5 L)
- dry with materialDry the extracts over magnesium sulfate
- filtrationfilter
- customevaporate to a brown solid
- customTriturate with diethyl ether