反应 #1597034

ord-47bc8e8ab3894df38d504e2b25ea6168

反应方程式

BrC1CCCCC1
Cyclohexyl bromide
[N-]=[N+]=[N-].[Na+]
sodium azide
CS(C)=O
DMSO
[N-]=[N+]=NC1CCCCC1
title compound
[N-]=[N+]=NC1CCCCC1
Cyclohexyl Azide

反应条件

温度
75°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was then cooled with an ice-bath
  2. 2
    其他quenched by the addition of water (75 mL)
  3. 3
    萃取extracted with diethyl ether (3×125 mL)
  4. 4
    洗涤The combined organic layers were washed with brine (75 mL)
  5. 5
    干燥dried (MgSO4)
  6. 6
    过滤filtered
  7. 7
    浓缩concentrated in vacuo

实验过程

Cyclohexyl bromide (2.74 mL, 0.023 mol) was added to a stirred solution of 0.5M sodium azide in DMSO (50 mL, 0.025 mol) at room temperature, under an atmosphere of nitrogen. The reaction mixture was heated to 75° C. behind a blast shield and stirred for 5 h. The reaction mixture was then cooled with an ice-bath, quenched by the addition of water (75 mL) and extracted with diethyl ether (3×125 mL). The combined organic layers were washed with brine (75 mL), dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a crude oil (2.4 g) which was used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08211894B2uspto-grants-2012_07