HRID270047
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
PROCEDURE
实验过程
A solution of 1′-benzyl-6-chloro-3,4-dihydrospiro[chromene-2,4′-piperidine] (1.63 g, 5.0 mmol) and 1-chloroethyl chloroformate (1.07 g, 7.5 mmol) in toluene (5 ml) was heated with reflux overnight. The solvent was removed i. vacuo, the oily residue dissolved in methanol (10 ml) and heated with reflux overnight. The solvent was removed in vacuo, and the residue treated with diethyl ether (50 ml). The white precipitate was collected by filtration, washed with diethyl ether and dried to afford the subtitle compound as white powder (0.58 g, 49%).
WORKUP
后处理
- temperaturewith reflux overnight
- customThe solvent was removed i
- dissolutionvacuo, the oily residue dissolved in methanol (10 ml)
- temperatureheated
- temperaturewith reflux overnight
- customThe solvent was removed in vacuo
- additionthe residue treated with diethyl ether (50 ml)
- filtrationThe white precipitate was collected by filtration
- washwashed with diethyl ether
- customdried