Sodium Hydroxide → 8-bromo-2,3,4,5-tetrahydro-1H-benzofuro[3,2-c]azepin-1-one
反応式
[Br:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]3[C:12](=[N:13]O)[CH2:11][CH2:10][CH2:9][C:7]=3[O:8][C:4]=2[CH:3]=1.[OH-:17].[Na+]>O>[Br:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]3[C:12](=[O:17])[NH:13][CH2:11][CH2:10][CH2:9][C:7]=3[O:8][C:4]=2[CH:3]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
A mixture of the product of step B (1.05 g, 3.74 mmol) and polyphosphoric acid (15 g) was heated to 110° C. for 5 h. After cooling to ambient temperature, the reaction mixture was diluted with water, basified with 10 N NaOH and filtered. The solid obtained was washed with water and dried in vacuo at 70° C. to give 8-bromo-2,3,4,5-tetrahydro-1H-benzofuro[3,2-c]azepin-1-one (858 mg, 82%) as a white solid: 1H NMR (DMSO-d6, 300 MHz) δ 8.06-7.95 (m, 2H), 7.86 (d, J=1.8 Hz, 1H), 7.45 (dd, J=8.4, 1.8 Hz, 1H), 3.28-3.20 (m, 2H), 3.15 (t, J=6.6 Hz, 2H), 2.07-1.93 (m, 2H).