HRID2112265

反应详情

EQUATION

反应方程式

HRID 2112265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.0 g of 1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one, 1.65 g of 2-methyl imidazole and 274 g of dipiperidinomethane were suspended in 30 ml of acetonitrile, and then 2 g of aluminum chloride was slowly added thereto. The reaction mixture was stirred under reflux for 10 hours. 150 ml dichloromethane and 50 ml of 1N aq. sodium hydroxide were added to the reaction mixture. The resulting organic layer was separated and dried over MgSO4, and then evaporated. The resulting solid was suspended in acetone and stirred for 3 hours, and then filtered and dried under a reduced pressure to give 2.05 g of title compound (yield 70%).

WORKUP

后处理

  1. temperatureunder reflux for 10 hours
  2. customThe resulting organic layer was separated
  3. dry with materialdried over MgSO4
  4. customevaporated
  5. stirringstirred for 3 hours
  6. filtrationfiltered
  7. customdried under a reduced pressure