HRID2058424

反应详情

EQUATION

反应方程式

HRID 2058424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated
  2. temperatureunder reflux for 19 hours
  3. filtrationthe suspension filtered and to the filtrate
  4. additionwas added a solution of oxalic acid (6.25%) in tetrahydrofuran (36 ml.)
  5. customThe solid which separated on trituration
  6. filtrationwas filtered
  7. washwashed with tetrahydrofuran
  8. customdried