(2-Amino-4-methoxyphenyl)methanol → 2-Amino-4-methoxybenzaldehyde

HRID 524071

反応式

HRID 524071 の反応式
[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

反応物 1

HCID 45090899(2-Amino-4-methoxyphenyl)methanol

生成物 1

HCID 3235032-Amino-4-methoxybenzaldehyde収率 35.3%

試薬・触媒・溶媒 2

HCID 160959Manganese oxide触媒HCID 6344Dichloromethane溶媒

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

  1. filtrationThe solid was filtered off
  2. concentrationthe filtrate was concentrated
  3. 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-bb2fe668888f4e2689fdc4ae23fd131e
出典データセット
uspto-grants-2016_05
特許番号
US09340514B2

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