反应详情

A mixture of 29 g of 6,7-dichloro-5-methoxy-2-n-propylbenzo[b]thiophene and 280 g of pyridine hydrochloride is heated at 190° for 5 hrs and allowed to cool. The reaction mixture is poured into 300 ml of water and extracted with three 33-ml portions of ether. The ether extracts are washed with 500 ml of 2N hydrochloric acid, water, dried over anhydrous magnesium sulfate-charcoal, filtered and evaporated to give an oil. Crystallization of the oil with hexane followed by recrystallization from hexane give 15.5 g of 6,7-dichloro-5-hydroxy-2-n-propylbenzo[b]thiophene, mp 50°-51°.

1. temperatureis heated at 190° for 5 hrs
2. temperatureto cool
3. extractionextracted with three 33-ml portions of ether
4. washThe ether extracts are washed with 500 ml of 2N hydrochloric acid, water
5. dry with materialdried over anhydrous magnesium sulfate-charcoal
6. filtrationfiltered
7. customevaporated
8. customto give an oil
9. customCrystallization of the oil with hexane
10. customfollowed by recrystallization from hexane