O-Methylhydroxylamine hydrochloride → HCID 86093123、化合物
反応式
[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13](=O)[CH3:14])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl.[CH3:17][O:18][NH2:19]>N1C=CC=CC=1.C(OCC)(=O)C>[CH3:17][O:18][N:19]=[C:13]([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1)[CH3:14]参加物
5
実験手順
A mixture of Example 49A (1.22 g, 5.94 mmol) and methoxyamine hydrochloride (550 mg, 6.59 mmol) in pyridine (20 mL) was stirred at room temperature for 12 h. The reaction was diluted with ethyl acetate and washed sequentially with 3 N HCl, 1 N HCl and brine. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated to dryness under reduced pressure to give 1.3 g of the title compound. MS (ESI+) m/z 235 (M+H)+.
後処理
- washwashed sequentially with 3 N HCl, 1 N HCl and brine
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-c8ba335ca5ed4a5ba5d22c9fd6b9ecaa
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07241776B2
反応ノート
読み込み中…