反応式
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[CH2:10][OH:11]>ClCCl.[O-2].[Mn+2]>[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[CH:10]=[O:11]参加物
4
実験手順
A mixture of (2-amino-4-methoxyphenyl)methanol (20 g, 131.0 mmol) and manganese oxide (68 g, 786.0 mmol) in dichloromethane (300 mL) was stirred at RT overnight. LCMS showed the reaction was completed. The solid was filtered off, and the filtrate was concentrated. The residue was purified by silica gel chromatography (petroleum ether:ethyl acetate=6:1) to give the title compound (7 g, 35%) as a yellow solid. MS (ES+) C8H9NO2 requires: 151. Found: 152 [M+H]+.
後処理
- filtrationThe solid was filtered off
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel chromatography (petroleum ether:ethyl acetate=6:1)
出典と根拠
- ORDレコード
- ord-3c4619a69ebf425f9c1b1b4a1936e555
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09126951B2
関連ノート
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