1-Indanone, 4-bromo- → 4-Bromoindan-1-one O-methyloxime
반응식
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][C:6]2=O.Cl.[CH3:13][O:14][NH2:15]>N1C=CC=CC=1>[CH3:13][O:14][N:15]=[C:6]1[C:7]2[C:3](=[C:2]([Br:1])[CH:10]=[CH:9][CH:8]=2)[CH2:4][CH2:5]1참가 물질
4
실험 절차
4-Bromoindan-1-one (5.08 g, 24.1 mmol) was added to a mixture of methoxyamine hydrochloride (2.21 g, 26.5 mmol) in pyridine (40 mL) under nitrogen atmosphere and stirred overnight at ambient temperature. The reaction mixture was concentrated, added ethyl acetate (200 mL), washed with 3N hydrochloric acid (200 mL), dried with brine and anhydrous sodium sulfate, and concentrated. Obtained 4-bromoindan-1-one O-methyloxime (5.66 g, 98%) as an orange liquid. MS (DCI/NH3) m/z: 239.94 [M+H]+. 1H NMR (DMSO-d6) □: 2.83 (m, 2H), 2.96 (m, 2H), 3.91 (s, 3H), 7.25 (t, 1H), 7.56 (d, 1H), 7.60 (d, 1H).
후처리
- concentrationThe reaction mixture was concentrated
- additionadded ethyl acetate (200 mL)
- washwashed with 3N hydrochloric acid (200 mL)
- dry with materialdried with brine and anhydrous sodium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-884712706ee14c21a8251d7c2c6f3e3d
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08487116B2
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