反応 #41537

反応方程式

chloromethyl methyl ether

sodium hydride

tetrahydrofuran

ethyl 3-bromo-4-hydroxybenzoate

→

compound

ethyl 3-bromo-4-methoxymethoxybenzoate

溶媒

ethyl acetate

反応条件

後処理

1. 1
   その他produced
2. 2
   温度437, with cooling with ice
3. 3
   その他the reaction liquid
4. 4
   その他the reaction liquid
5. 5
   workup.STIRRINGwas stirred overnight at room temperature
6. 6
   その他The reaction liquid
7. 7
   洗浄washed with water
8. 8
   抽出the aqueous layer was extracted with ethyl acetate
9. 9
   乾燥dried with anhydrous magnesium sulfate
10. 10
    その他The solvent was evaporated away under reduced pressure
11. 11
    ろ過taken out through filtration

実験手順

5.5 g of sodium hydride was added to a tetrahydrofuran (300 ml) solution of 20.5 g of ethyl 3-bromo-4-hydroxybenzoate produced according to the method described in Monatsh. Chem.; 22; 1901; 437, with cooling with ice, and the reaction liquid was stirred for 30 minutes, and then, at the same temperature, 10 ml of chloromethyl methyl ether was added to the reaction liquid, and the reaction liquid was stirred overnight at room temperature. The reaction liquid was diluted with ethyl acetate, and washed with water, and the aqueous layer was extracted with ethyl acetate, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting solid was suspended in hexane and then taken out through filtration to obtain the entitled compound as a white solid.

出典