HRID2058424
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 mixture of 3-[3-[(1-piperidinyl)methyl]phenoxy]propanamine (4.97 g.) and 1,1-bis-(methylthio)-2-nitroethene (6.61 g.) in tetrahydrofuran (100 ml.) was heated under reflux for 19 hours. A solution of oxalic acid (6.25%) in tetrahydrofuran (4 ml.) was added, the suspension filtered and to the filtrate was added a solution of oxalic acid (6.25%) in tetrahydrofuran (36 ml.). The solid which separated on trituration was filtered, washed with tetrahydrofuran and dried to give the title compound (7.36 g.), m.p. 71°-75°.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 19 hours
- filtrationthe suspension filtered and to the filtrate
- additionwas added a solution of oxalic acid (6.25%) in tetrahydrofuran (36 ml.)
- customThe solid which separated on trituration
- filtrationwas filtered
- washwashed with tetrahydrofuran
- customdried