反应详情

tert-Butyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate (12.26 g, 48.4 mmol) was dissolved in DCM (150 ml), and pyridine (6.0 ml, 74 mmol) was added thereto. A solution of 3,4-dichlorobenzenesulfonyl chloride (8.4 ml, 54 mmol) was then added, and the mixture was heated for 17 h under reflux and then cooled to room temperature. Water was added (100 ml), and stirring was carried out overnight at room temperature. The phases were then separated (pH organic phase≈2), washed with saturated NaHCO3 solution, dried (sodium sulfate) and concentrated in vacuo.

1. temperaturethe mixture was heated for 17 h
2. temperatureunder reflux
3. customThe phases were then separated (pH organic phase≈2),
4. washwashed with saturated NaHCO3 solution
5. dry with materialdried (sodium sulfate)
6. concentrationconcentrated in vacuo