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

HRID 1383304

반응식

HRID 1383304 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-af568a6e2a924fa6b7619dfae69a4515
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255310B1

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