反应详情

To a mixture of 6,7-dichloro-5-hydroxy-α-ethylbenzo[b]thiophene-2-methanol and 200 ml of 2-butanone is added a mixture of 7.35 g of ethyl bromoacetate in 100 ml of 2-butanone, followed by 7.4 g of potassium carbonate and 3.3 ml of sieve-dried dimethylformamide. The reaction mixture is stirred at 95°-100° for 3 hrs, allowed to cool and filtered. To the filtrate is added 100 ml of water and the mixture is extracted with ethyl ether. The organic layers are washed, dried over anhydrous magnesium sulfate, filtered and the solvent removed to give an oil which solidifies on cooling. Recrystallization from ethyl ether and hexane gives 10 g of ethyl [(6,7-dichloro-2-(1-hydroxypropyl]benzo[b]thien-5-yl]oxy]acetate, mp 69°-70°.

1. additionis added
2. temperatureto cool
3. filtrationfiltered
4. additionTo the filtrate is added 100 ml of water
5. extractionthe mixture is extracted with ethyl ether
6. washThe organic layers are washed
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customthe solvent removed
10. customto give an oil which
11. temperatureon cooling
12. customRecrystallization from ethyl ether and hexane