Chloromethyl Methyl Ether → 3-Methoxy-4-methoxymethoxy-benzonitrile

HRID 1016615

反応式

HRID 1016615 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[O:10][CH3:11].C(N(C(C)C)CC)(C)C.Cl[CH2:22][O:23][CH3:24]>C(Cl)Cl>[CH3:11][O:10][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:2]=1[O:1][CH2:22][O:23][CH3:24])[C:6]#[N:7]

参加物

5

反応物 3

HCID 7864Chloromethyl Methyl EtherHCID 781354-Hydroxy-3-methoxybenzonitrileHCID 81531Diisopropylethylamine

生成物 1

HCID 222583333-Methoxy-4-methoxymethoxy-benzonitrile収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 4-hydroxy-3-methoxy-benzonitrile (11, 1.5 g, 10 mmol) and diisopropylethylamine (2.7 mL, 15 mmol) in CH2Cl2 (50 mL) was treated with chloromethylmethylether (0.92 mL, 12 mmol) and stirred for 3 h. After diluted with CH2Cl2, the mixture was washed with H2O, dried over MgSO4 and concentrated in vacuo. The residue was purified by flash column chromatography over silica gel using EtOAc:Hex (1:2) as eluant to give 12 as white solid (1.54 g, 80%).

後処理

  1. washthe mixture was washed with H2O
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by flash column chromatography over silica gel

出典と根拠

ORDレコード
ord-de16a529e10344f6a3f98e7a744a07a7
出典データセット
uspto-grants-2002_11
特許番号
US06476076B1

関連ノート

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