反应详情

In a mixed solvent of 30 ml of methanol and 20 ml of chloroform was dissolved 6 g of 2-tert-butoxycarbonyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-carboxylic acid ethyl ester and 4 ml of an aqueous solution of 5N sodium hydroxide was further added thereto, and then the solution was refluxed for 5 hours. The solvents were distilled off under reduced pressure and 300 ml of 5% citric acid and 300 ml of chloroform were added to the residue. The chloroform layer was washed with a saturated aqueous sodium chloride solution and then dried by sodium sulfate. After distilling off chloroform under reduced pressure, the residue formed was recrystallized from a mixture of chloroform and hexane to provide 4.15 g (yield of 75%) of 2-tert-butoxycarbonyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-3-carboxylic acid.

1. additionwas further added
2. temperaturethe solution was refluxed for 5 hours
3. distillationThe solvents were distilled off under reduced pressure and 300 ml of 5% citric acid and 300 ml of chloroform
4. additionwere added to the residue
5. washThe chloroform layer was washed with a saturated aqueous sodium chloride solution
6. dry with materialdried by sodium sulfate
7. distillationAfter distilling off chloroform under reduced pressure
8. customthe residue formed
9. customwas recrystallized from a mixture of chloroform and hexane