HRID863064

反应详情

EQUATION

反应方程式

HRID 863064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of (R)-5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl methanesulfonate (54.0 g), prepared as in Example 7, and lithium azide (15.8 g, 0.322 mol) in 400 mL of DMF was stirred under argon at 50° C. for 16 hours. The reaction was quenched with 200 mL of water and the mixture extracted with 1 L of pentane. The extract was washed with 50 mL of water and dried over magnesium sulfate. Evaporation under reduced pressure at 35° C. gave crude (S)-2-azido-5,7-difluoro-1,2,3,4-tetrahydronaphthalene as a yellow oil residue (59.8 g).

WORKUP

后处理

  1. customThe reaction was quenched with 200 mL of water
  2. extractionthe mixture extracted with 1 L of pentane
  3. washThe extract was washed with 50 mL of water
  4. dry with materialdried over magnesium sulfate
  5. customEvaporation under reduced pressure at 35° C.