反应详情

To a solution of 7-bromo-4-(chloromethyl)-5-methyl-2,3-dihydrobenzo[b]oxepine from step H7 (2.05 g, 7.13 mmol) in ethanol (75 mL) was added thiourea (0.651 g, 8.55 mmol). The mixture was refluxed for 3 h. A white solid precipitated. The solvent was removed. The solid residue was washed with hexanes and dried in vacuo to give a (7-bromo-5-methyl-2,3-dihydrobenzo[b]oxepin-4-yl)methyl carbamimidothioate hydrochloride (2.64 g, 7.26 mmol, 102% yield). The crude mixture was used in the next step without further purification. 1H NMR (500 MHz, methanol-d4) δ 7.48 (d, J=2.4 Hz, 1H), 7.43-7.36 (m, 1H), 6.97 (d, J=8.5 Hz, 1H), 4.53 (t, J=6.3 Hz, 2H), 4.25 (s, 2H), 2.34 (t, J=6.1 Hz, 2H), 2.18 (s, 3H).

1. temperatureThe mixture was refluxed for 3 h
2. customA white solid precipitated
3. customThe solvent was removed
4. washThe solid residue was washed with hexanes
5. customdried in vacuo