반응 #72640
ord-35795869fc134710aa3df281aef8b985
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과the precipitate was filtered
- 2세척washed with dioxane
- 3농축The filtrate was concentrated under reduced pressure
- 4기타the residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (3:7)
실험 절차
A solution of 2-amino-6-methylbenzonitrile (1.32 g, 10 mmol) and sulfamide (4.81 g, 50 mmol) in dry 1,4-dioxane (50 mL) was refluxed under nitrogen for 3 days. After the reaction mixture was cooled down to room temperature, the precipitate was filtered and washed with dioxane. The filtrate was concentrated under reduced pressure, and the residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (3:7) to give the title compound as a pale-white solid. 1H NMR (400 MHz, DMSO-d6) δ2.44 (s, 3H), 7.19-7.21 (m, 3H), 7.39-7.41 (d, J=8.4 Hz, 1H), 7.53 (t, J=8.0 Hz, 1H), 9.41 (s, 1H).