反应 #50111

反应方程式

epoxide

1,3,3-trichloro-2-methyl-7-oxabicyclo[4.1.0]heptane

HCl

→

phenol

收率 89.2%

3-chloro-2-methylphenol

收率 89.2%

溶剂

DMF

反应条件

后处理

1. 1
   温度to reflux for 3 h
2. 2
   萃取extracted with ether (4×25 cm3)
3. 3
   干燥dried over MgSO4
4. 4
   过滤filtered
5. 5
   其他evaporated down
6. 6
   其他The crude product obtained
7. 7
   其他was purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95)

实验过程

2 g (9.28 mmol) of epoxide 2h in solution in 5 cm3 of anhydrous DMF were heated to reflux for 3 h. The solution was acidified (pH=1) with 3N HCl, extracted with ether (4×25 cm3), dried over MgSO4, filtered and evaporated down. The crude product obtained was purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95). 1.18 g of phenol 4e were obtained (macrobore GC purity>96%). The yield of compound 4e was 89%.

来源