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

HRID 844008

反応式

HRID 844008 の反応式
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]

参加物

5

反応物 3

HCID 13387N-methyl-2-pyrrolidoneHCID 27735853-Chloro-4-fluoroanisoleHCID 178418546HCID 178418546、化合物2 回

生成物 1

HCID 27745462-Fluoro-5-methoxybenzonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-3975cb63a80e47fcaea38a24e043d76d
出典データセット
uspto-grants-2002_04
特許番号
US06380218B1

関連ノート

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