Water → 5-Methoxy-2-(methylsulfanyl)benzonitrile

HRID 1013972

反応式

HRID 1013972 の反応式
F[C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[C:4]#[N:5].[CH3:12][S-:13].[Na+].O>CN(C)C=O>[CH3:11][O:10][C:7]1[CH:8]=[CH:9][C:2]([S:13][CH3:12])=[C:3]([CH:6]=1)[C:4]#[N:5]

参加物

5

反応物 3

HCID 962WaterHCID 27745462-Fluoro-5-methoxybenzonitrileHCID 4378561Sodium methanethiolate

生成物 1

HCID 668777365-Methoxy-2-(methylsulfanyl)benzonitrile収率 70%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(Step 1) A mixture of 2-fluoro-5-methoxybenzonitrile (10 g) and sodium methanethiolate (5.1 g) was stirred in N,N-dimethylformamide (20 ml) at 60° C. for 3 hr. The reaction solution was treated with water, and extracted with ethyl acetate. The extract was washed successively with 1N hydrochloric acid, aqueous sodium hydrogen carbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was crystallized from ethyl acetate-hexane to give 5-methoxy-2-(methylsulfanyl)benzonitrile (8.3 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed successively with 1N hydrochloric acid, aqueous sodium hydrogen carbonate solution and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe obtained residue was crystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-95a5a53467594f6a9ff36021ec546772
出典データセット
uspto-grants-2011_07
特許番号
US07982044B2

関連ノート

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