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

HRID 48978

反応式

HRID 48978 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2faec26a94d54e92a133e6d5e439322b
出典データセット
uspto-grants-2004_03
特許番号
US06706663B2

関連ノート

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