HRID2177489

反应详情

EQUATION

反应方程式

HRID 2177489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To 2.06 ml of a 2.5M lithium aluminium hydride solution in tetrahydrofuran cooled to 0° C. was added dropwise a solution of 452 mg (2.15 mmol) rac-5-amino-5-cyclohexyl-1-methyl-piperidin-2-one in 6 ml tetrahydrofuran. Then the solution was heated to 65° C. for 1 hour. The turbid reaction solution was cooled with an ice bath and below 12° C. were added drop-wise 0.13 ml water, 0.32 ml 2N NaOH and further 0.19 ml water. The suspension was diluted with tert-butyl methyl ether, dried over sodium sulfate, filtered and evaporated: 368 mg title compound were obtained as colourless oil which was used without purification for the next step.

WORKUP

后处理

  1. customThe turbid reaction solution
  2. temperaturewas cooled with an ice bath and below 12° C.
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated