HRID473331

反应详情

EQUATION

反应方程式

HRID 473331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

1,1-Dimethylethyl (3S)-3-fluoro-3-({[(trifluoromethyl)sulfonyl]oxy}methyl)-1-piperidinecarboxylate (1 wt) is dissolved in N,N,-dimethylformamide (3 vol) at 20° C. and sodium azide (1.1 eq, 0.20 wt) is added. The resulting suspension is stirred at 20-30° C. for 6 h. TBME (5 vol) and water (9 vol) are added. The mixture is stirred for 5 min and the layers are separated. The aqueous phase is extracted with TBME (5 vol) and the TBME phases are combined. The combined organics are washed with water (2×5 vol), filtered and concentrated under reduced pressure to give the title compound as an orange oil.

WORKUP

后处理

  1. stirringThe mixture is stirred for 5 min
  2. customthe layers are separated
  3. extractionThe aqueous phase is extracted with TBME (5 vol)
  4. washThe combined organics are washed with water (2×5 vol)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure