Water → 3-Methanesulfonyl-2-(2,4,6-trimethylphenyl)acrylonitrile

HRID 1383304

反応式

HRID 1383304 の反応式
O[CH:2]=[C:3]([C:6]1[C:11]([CH3:12])=[CH:10][C:9]([CH3:13])=[CH:8][C:7]=1[CH3:14])[C:4]#[N:5].[CH3:15][S:16](Cl)(=[O:18])=[O:17].O>N1C=CC=CC=1>[CH3:15][S:16]([CH:2]=[C:3]([C:6]1[C:11]([CH3:12])=[CH:10][C:9]([CH3:13])=[CH:8][C:7]=1[CH3:14])[C:4]#[N:5])(=[O:18])=[O:17]

参加物

5

反応物 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 701428183-Hydroxy-2-(2,4,6-trimethylphenyl)acrylonitrile

生成物 1

HCID 536820093-Methanesulfonyl-2-(2,4,6-trimethylphenyl)acrylonitrile収率 105.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of intermediate 1 (1 g) in 10 ml pyridine was cooled to 0° C. under nitrogen and then treated with methanesulfonyl chloride (0.67 g) with good stirring. The solution was allowed to come to room temperature and stirred for 1 hour. The reaction mixture was poured into water and extracted with ethyl acetate. The organic phase was washed with 1M HCl, water and brine, dried (MgSO4) and concentrated to give 3-methanesulfonyl-2-(2,4,6-trimethylphenyl)acrylonitrile (intermediate 2) as a brown solid (1.4 g).

後処理

  1. customto come to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed with 1M HCl, water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-af568a6e2a924fa6b7619dfae69a4515
出典データセット
uspto-grants-2001_07
特許番号
US06255310B1

関連ノート

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