Pyridine → 3-(3,5-Dimethylpyrazol-1-yl)-5-nitro-1,2-benzisothiazole

HRID 48978

반응식

HRID 48978 반응식
Cl[C:2]1[C:6]2[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=2[S:4][N:3]=1.[CH3:14][C:15]1[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=1.N1C=CC=CC=1>C(OCC)(=O)C>[CH3:14][C:15]1[CH:19]=[C:18]([CH3:20])[N:17]([C:2]2[C:6]3[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=3[S:4][N:3]=2)[N:16]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 62103,5-DimethylpyrazoleHCID 1980981,2-Benzisothiazole, 3-chloro-5-nitro-

생성물 1

HCID 206342663-(3,5-Dimethylpyrazol-1-yl)-5-nitro-1,2-benzisothiazole수율 43.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 3-chloro-5-nitrobenzisothiazole (5.3 g, mmol), 3,5-dimethylpyrazole (2.40 g, 25.0 mmol) and pyridine is stirred overnight at reflux, cooled to room temperature and diluted with ethyl acetate. The resultant mixture is filtered and the filtrate is washed with three portions of 10% hydrochloric acid and one portion of water. The organic layer is dried over anhydrous magnesium sulfate and concentrated in vacuo to afford the title compound (2.85 g, 43.8%) which is identified by NMR spectral analysis.

후처리

  1. temperatureat reflux
  2. filtrationThe resultant mixture is filtered
  3. washthe filtrate is washed with three portions of 10% hydrochloric acid and one portion of water
  4. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2faec26a94d54e92a133e6d5e439322b
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706663B2

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