HRID34712
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 8.0 g of N-(2-chloroethyl)piperidine hydrochloride and 0.5 g of sodium iodide in 60 ml of methanol which contained 40% of methylamine was reacted at 70° C. in a sealed tube for 20 hours. After allowing the reaction mixture to cool down, the reaction mixture was concentrated under reduced pressure. The residue was added with ether, followed by a further addition of 10 g of ground sodium hydroxide. The resulting mixture was stirred for 2 hours. The insoluble material was filtered off and the filtrate was concentrated under the atmospheric pressure. The residue was distilled under reduced pressure to give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%).
WORKUP
后处理
- customwas reacted at 70° C. in a sealed tube for 20 hours
- temperatureto cool down
- concentrationthe reaction mixture was concentrated under reduced pressure
- additionThe residue was added with ether
- additionfollowed by a further addition of 10 g of ground sodium hydroxide
- filtrationThe insoluble material was filtered off
- concentrationthe filtrate was concentrated under the atmospheric pressure
- distillationThe residue was distilled under reduced pressure
- customto give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%)