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

HRID 1016615

반응식

HRID 1016615 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 222583333-Methoxy-4-methoxymethoxy-benzonitrile수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-de16a529e10344f6a3f98e7a744a07a7
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06476076B1

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