1-Indanone, 4-bromo- → 4-Bromoindan-1-one O-methyloxime
反応式
[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]1参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-cec9473b9a674e208ae9ac53f7575116
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071762B2
反応ノート
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