反应详情

A mixture of 11.5 g of 6,7-dichloro-5-hydroxy-2-n-propylbenzo[b]thiophene, 8.82 g of ethyl bromoacetate, 7.52 g of potassium carbonate, 135 ml of 2-butanone and 9 ml of dimethylformamide is stirred for 3 days. The reaction mixture is filtered and 100 ml of water and 100 ml of ether are added. The layers are separated and the aqueous layer is extracted 2 times with 100-ml portions of ether. The combined organic layers are dried, filtered and the filtrate is evaporated to give an oil which crystallizes from hexane. Recrystallization from ether-hexane gives 9 g of ethyl [(6,7-dichloro-2-n-propylbenzo[b]thien-5-yl)oxy]acetate, mp 62°-63°.

1. filtrationThe reaction mixture is filtered
2. addition100 ml of water and 100 ml of ether are added
3. customThe layers are separated
4. extractionthe aqueous layer is extracted 2 times with 100-ml portions of ether
5. customThe combined organic layers are dried
6. filtrationfiltered
7. customthe filtrate is evaporated
8. customto give an oil which
9. customcrystallizes from hexane
10. customRecrystallization from ether-hexane