Water → 4-(Methylsulfonyl)benzonitrile

HRID 901900

反応式

HRID 901900 の反応式
[OH:1]OS([O-])=O.[K+].[CH3:7][S:8][C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1.[OH2:17]>CO>[CH3:7][S:8]([C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1)(=[O:1])=[O:17]

参加物

5

反応物 3

HCID 962Water2 回HCID 5909604-(Methylthio)benzonitrileHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 5199814-(Methylsulfonyl)benzonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of oxone (18.42 g, 0.03 mol) in water (70 ml) was added dropwise to the vigorous stirred solution of 4-methylthiobenzonitrile (1.49 g, 0.01 mol) in methanol (50 ml) at 20° C. and stirring was continued for three hours. The reaction mixture was diluted with water (50 ml) and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous sodium sulphate and concentrated under reduced pressure to finish the title compound (1.3 g, 72.2%), mp 145-149° C. The compound was used with out any purification for the next step. 1H-NMR (CDCl3):δ 3.1 (s, 3H), 7.8-7.9 (d, 2H), 8.08-8.1 (d, 2H).

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe ethyl acetate extract
  3. washwas washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. concentrationconcentrated under reduced pressure
  6. customThe compound was used with out any purification for the next step

出典と根拠

ORDレコード
ord-e49c99a73935496d9b326a44e8837331
出典データセット
uspto-grants-2008_04
特許番号
US07365069B2

関連ノート

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