1,3-Dibromopropane → 2H-1,4-Benzoxazine, 4-(3-bromopropyl)-3,4-dihydro-
반응식
[O:1]1[CH2:6][CH2:5][NH:4][C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]1=2.[Br:11][CH2:12][CH2:13][CH2:14]Br.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C.C(OCC)(=O)C>[O:1]1[CH2:6][CH2:5][N:4]([CH2:14][CH2:13][CH2:12][Br:11])[C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]1=2참가 물질
6
반응 조건
- 온도
- 70 °C
실험 절차
A mixture of 3,4-dihydro-2H-benzo[b][1,4]oxazine (3.0 g, 1 eq, 22.2 mmol), 1,3-dibromopropane (22.5 ml, 10 eq, 222 mmol) and anhydrous sodium carbonate (7.05 g, 3 eq, 66.6 mmol) in dry DMF (200 ml) was heated at 70° C. for 16 h. The reaction mixture was diluted with ethyl acetate and washed with water and brine. The residue was chromatographed using ethyl acetate and hexane to yield the title compounds as liquid mass (2.6 g, 47%).
후처리
- washwashed with water and brine
- customThe residue was chromatographed
출처 및 근거
- ORD 기록
- ord-538ea71e18814810a68e0e9c5a8608eb
- 출처 데이터셋
- uspto-grants-2008_04
- 특허 번호
- US07365064B2
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