Water → 4-Fluoro-3-methoxymethoxybenzonitrile

HRID 1255618노트

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HRID 1255618 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[OH:10].C(N(C(C)C)CC)(C)C.[CH3:20][O:21][CH2:22]Cl.O>ClCCl>[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[O:10][CH2:20][O:21][CH3:22]

참가 물질

6

반응물 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 207769814-Fluoro-3-hydroxybenzonitrile

생성물 1

HCID 674399604-Fluoro-3-methoxymethoxybenzonitrile수율 100.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-fluoro-3-hydroxybenzonitrile (25.0 g, 182 mmol), diisopropylethylamine (47.7 mL, 273 mmol) in dichloromethane (530 mL) was added chloromethyl methyl ether (16.6 mL, 219 mmol) dropwise at 0° C., and the mixture was stirred at room temperature overnight. Water was added, and the mixture was extracted with dichloromethane. The organic layer was washed with brine and dried on anhydrous sodium sulfate. The solvent was removed under reduced pressure to give 4-fluoro-3-methoxymethoxybenzonitrile (33.0 g, quant.), which was used for the next step without purification.

후처리

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe organic layer was washed with brine
  3. dry with materialdried on anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-2f232ce6d0664ccebece5ce3c1d1e6b5
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461135B2

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