反应 #632006

反应方程式

N-tert-butyl-(3-chloro)propylsulfonamide

n-butyllithium

→

desired product

收率 56.4%

Cyclopropanesulfonic Acid Tert-Butylamide

收率 56.4%

溶剂

THF

反应条件

后处理

1. 1
   浓缩concentrated in vacuo
2. 2
   其他The concentrate was partitioned between ethyl acetate and water (200 mL, 200 mL)
3. 3
   洗涤The organic phase was washed with brine
4. 4
   干燥dried over Na2SO4
5. 5
   过滤filtered
6. 6
   浓缩concentrated in vacuo
7. 7
   其他The concentrate was recrystallized from hexane

实验过程

To a solution of N-tert-butyl-(3-chloro)propylsulfonamide (2.14 g, 10.0 mmol) in THF (100 mL) was added n-butyllithium (2.5M in hexane, 8.0 mL, 20.0 mmol) at −78° C. The reaction mixture was warmed to room temperature over a period of 1 hour and concentrated in vacuo. The concentrate was partitioned between ethyl acetate and water (200 mL, 200 mL). The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The concentrate was recrystallized from hexane to provide the desired product as a white solid (1.0 g, 56%). 1H NMR (CDCl3) δ 0.98-1.00 (m, 2H), 1.18-1.19 (m, 2H), 1.39 (s, 9H), 2.48-2.51 (m, 1H), 4.19 (br, 1H).

来源