反应 #51973

反应方程式

MgSO4

N-chlorosuccinimide

2-{1-[(Triisopropylsilyl)oxy]vinyl}pyrimidine

ether

→

product

2-{2-Chloro-1-[(triisopropylsilyl)oxy]ethenyl}pyrimidine

溶剂

THF

hexane

反应条件

后处理

1. 1
   温度then heated at 65° for 5 hr
2. 2
   温度After cooling
3. 3
   洗涤washed
4. 4
   干燥The organic layer was dried over sodium sulfate
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他to leave an amber oil
8. 8
   过滤filtered
9. 9
   其他Evaporation

实验过程

N-chlorosuccinimide (9.97 g, 74.7 mmol) was added to a solution of 2-{1-[(Triisopropylsilyl)oxy]vinyl}pyrimidine (17.3 g, 62.2 mmol) in dry THF (120 ml) under N2 then heated at 65° for 5 hr. After cooling, ether (275 ml) was added and then washed with sat sodium bicarbonate solution (2×100 ml). The organic layer was dried over sodium sulfate, filtered and evaporated to leave an amber oil. This oil was dissolved in hexane (250 ml), treated with MgSO4 and filtered. Evaporation afforded the product as a yellow oil in quantitative yield.

来源