反应 #1166462

反应方程式

3-methoxy-4-hydroxy-7-acetoxy-2H-l-benzopyran-2-one

benzyl bromide

sodium carbonate

→

title compound

收率 37.0%

3-methoxy-4-benzyloxy-7-acetoxy-2H-1-benzopyran-2-one

收率 37.0%

溶剂

DMF

反应条件

后处理

1. 1
   过滤The solid in the reaction mixture was filtered off
2. 2
   workup.ADDITIONthe filtrate was poured into 200 ml of water
3. 3
   萃取extracted with 500 ml of benzene
4. 4
   浓缩The organic layler was concentrated in vacuo
5. 5
   干燥after drying over magnesium sulfate
6. 6
   其他to give oily residue
7. 7
   其他The residue was purified on silica gel column chromatography (eluent: benzene/ethyl acetate=7/3)

实验过程

To a mixture of 8.11 g of 3-methoxy-4-hydroxy-7-acetoxy-2H-l-benzopyran-2-one (27.8 mmol) and 5.71 g of benzyl bromide (33.4mmol) in 50 ml of DMF was added 4.61 g of sodium carbonate (33.4 mmol) under argon atmosphere, then the mixture was stirred at 50° for 2 hours. The solid in the reaction mixture was filtered off, the filtrate was poured into 200 ml of water and extracted with 500 ml of benzene. The organic layler was concentrated in vacuo after drying over magnesium sulfate to give oily residue. The residue was purified on silica gel column chromatography (eluent: benzene/ethyl acetate=7/3) to give 3.50 g of the title compound. (yield=33%)

来源