N-methyl-2-pyrrolidone → 2-Fluoro-5-methoxybenzonitrile

HRID 844008

반응식

HRID 844008 반응식
Cl[C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[F:10].[C:11]([Cu])#[N:12].CN1CCCC1=O>C(Cl)Cl>[F:10][C:3]1[CH:4]=[CH:5][C:6]([O:8][CH3:9])=[CH:7][C:2]=1[C:11]#[N:12]

참가 물질

5

반응물 3

HCID 13387N-methyl-2-pyrrolidoneHCID 27735853-Chloro-4-fluoroanisoleHCID 178418546HCID 178418546, 화합물2회

생성물 1

HCID 27745462-Fluoro-5-methoxybenzonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-Chloro-1-fluoro-4-methoxy-benzene (10.4 grams, 65.0 mmole), CuCN (6.4 grams, 71.0 mmole) and N-methylpyrrolidinone (100 ml) was refluxed for 18 hours. An additional 2.3 g CuCN was added, and the mixture was refluxed for 40 hours. The mixture was poured into 300 ml ice water and stirred for 10 minutes. This was poured into 100 ml methylene chloride and the layers were separated. The mixture was washed with water, dried over MgSO4, filtered, and concentrated to a solid (2.8 g). MW 137.12; MS (m/e) 137(M+).

후처리

  1. temperaturethe mixture was refluxed for 40 hours
  2. customthe layers were separated
  3. washThe mixture was washed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to a solid (2.8 g)

출처 및 근거

ORD 기록
ord-3975cb63a80e47fcaea38a24e043d76d
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380218B1

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