反应 #1518218
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09265763B2
反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5 g of 4-(bromomethyl)benzenesulfonyl chloride (18.6 mmol, 1 eq.) were dissolved under argon atmosphere in 82.5 ml of dichloromethane and cooled down at −10° C. internal temperature. A solution of 1.29 ml cyclopropanamine (18.6 mmol, 1 eq.) and 2.59 ml of triethylamine (18.6 mmol, 1 eq.) in 82.5 ml of dichloromethane were added dropwise at −10° C. internal temperature and stirred at this temperature for one hour. The reaction mixture was washed once with 1 M aqueous hydrogen solution and twice with distilled water. The organic layer was dried over sodium sulfate and concentrated in vacuo. The crude product contained a mixture of bromomethyl- and chloromethyl-substituents. The reaction mixture was washed once with 1 M aqueous hydrogen solution and twice with distilled water The organic layer was dried over sodium sulfate concentrated in vacuo a mixture of bromomethyl- and chloromethyl-substituents
来源 ID: ord-e00df9eb5ac44192ad6b97ae406f38f9