반응 #41537

반응 방정식

chloromethyl methyl ether

sodium hydride

tetrahydrofuran

ethyl 3-bromo-4-hydroxybenzoate

→

compound

ethyl 3-bromo-4-methoxymethoxybenzoate

용매

ethyl acetate

반응 조건

후처리

1. 1
   기타produced
2. 2
   온도437, with cooling with ice
3. 3
   기타the reaction liquid
4. 4
   기타the reaction liquid
5. 5
   workup.STIRRINGwas stirred overnight at room temperature
6. 6
   기타The reaction liquid
7. 7
   세척washed with water
8. 8
   추출the aqueous layer was extracted with ethyl acetate
9. 9
   건조dried with anhydrous magnesium sulfate
10. 10
    기타The solvent was evaporated away under reduced pressure
11. 11
    여과taken out through filtration

실험 절차

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.

출처