反応 #50111

反応方程式

epoxide

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

HCl

→

phenol

収率 89.2%

3-chloro-2-methylphenol

収率 89.2%

溶媒

DMF

反応条件

後処理

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

実験手順

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%.

出典