반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([O:22]C)[CH:20]=4)[CH2:15][CH2:14][N:13]=3)[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1>Br>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([OH:22])[CH:20]=4)[CH2:15][CH2:14][N:13]=3)[CH2:11][CH2:10][CH2:9]2)=[CH:6][CH:7]=1참가 물질
3
반응 조건
- 온도
- 120 °C
실험 절차
The crude 1-[1-(4-chlorophenyl)cyclobutyl]-7-methoxy-3,4-dihydroisoquinoline (10.25 g, 30.8 mmol) was treated with 47% aqueous hydrobromic acid (109 mL) and stirred at 120° C. for 4 h. The reaction mixture was cooled to room temperature. The aqueous layer was decanted. The crude product was treated with dichloromethan, methanol and water and the pH was adjusted to 10 with aqueous 1N sodium hydroxide solution. The product precipitated and the solid was collected by filtration. The product was washed with water and dried in vacuo at 30° C. Yield: 3.56 g (30.3, 12.38 mmol).
후처리
- temperatureThe reaction mixture was cooled to room temperature
- customThe aqueous layer was decanted
- additionThe crude product was treated with dichloromethan, methanol and water
- customThe product precipitated
- filtrationthe solid was collected by filtration
- washThe product was washed with water
- customdried in vacuo at 30° C
출처 및 근거
- ORD 기록
- ord-bf2362efddad4e5b9dec6b8942f56e9f
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08653100B2
연결된 노트
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