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With N-ethyl-N,N-diisopropylamine; In dichloromethane; at 20℃; for 16h;Product distribution / selectivity;
To 4-chloro-3-nitrobenzenesulfonyl chloride (1.0 g, 3.9 mmol) in dry DCM (10 ml_), was added 2,3,4,5-tetrahydro-1 H-benzo[b]azepine (0.57 g, 3.9 mmol). Diisopropylethylamine (1.3 ml_, 7.8 mmol) was added and the mixture was stirred at ambient temperature for 16 hrs. DCM (20 ml.) and 30 m L of water were added. The DCM layer was separated, washed with brine (20 mL x 2), dried over MgSO4 and evaporated to give 1-(3-nitro-4-chloro-benzenesulfonyl)-2,3,4,5-tetrahydro-1 H- benzo[b]azepine 4-1 as a yellow solid (1.3 g, 85% yield). MS: 367 (M+H)+; tR = 2.98 min (method 1 ).
With triethylamine; In dichloromethane; at 20℃; for 16h;Product distribution / selectivity;
1-(3-Nitro-4-chloro-benzenesulfonylV2.3,4.5-tetrahvdro-1 H-benzoMazepineTo 4-chloro-3-nitrobenzenesulfonyl chloride (2.56 g, 10 mmol ) in dry DCM (20 ml_) was added 2,3,4,5-tetrahydro-1 H-benzo[b]azepine (1.54 g, 10.5 mmol) and triethylamine (3.3 ml_, 25 mmol). The mixture was stirred at ambient temperature for 16 hrs. The mixture was then diluted with 40 ml_ of DCM and 30 ml. of water. The organic layer was separated, washed with brine (2 X 20 ml_), dried over MgSO4, and evaporated to afford 1-(3-nitro-4-chloro-benzenesulfonyl)-2,3,4,5-tetrahydro-1 H- benzo[b]azepine as a yellow solid (3.6 g).
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