Water → HCID 15230482、化合物

HRID 1464294ノート

反応式

HRID 1464294 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([SH:10])=[CH:6][CH:5]=1.[N+]([C:14]1[CH:15]=[C:16]2[C:20](=[CH:21][CH:22]=1)[C:19](=[O:23])[N:18]([CH2:24][C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[C:17]2=[O:31])([O-])=O.O>CN(C)C=O.C(OCC)(=O)C>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([S:10][C:22]2[CH:21]=[C:20]3[C:16](=[CH:15][CH:14]=2)[C:17](=[O:31])[N:18]([CH2:24][C:25]2[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=2)[C:19]3=[O:23])=[CH:6][CH:5]=1

参加物

7

反応物 4

HCID 962WaterHCID 7815p-ChlorothiophenolHCID 24758Sodium hydrideHCID 869878HCID 869878、化合物

生成物 1

HCID 15230482HCID 15230482、化合物収率 50.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

To a suspension of 42 mg of sodium hydride (about 60%) in 10 ml of dimethylformamide was added 150 mg of 4-chlorothiophenol, and the resultant mixture was stirred at 60° C. for 30 minutes and mixed with 300 mg of 5-nitro-2-(3-pyridylmethyl)-1H-isoindole-1,3 (2H)-dione. The mixture was heated at 120° C. for 8 hours under stirring, mixed with water and shaken with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, and the resultant, residue was chromatographed on a column of silica gel, eluting with chloroform to give 201 mg of the titled compound.

後処理

  1. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  2. concentrationconcentrated in vacuo
  3. customthe resultant, residue was chromatographed on a column of silica gel
  4. washeluting with chloroform

出典と根拠

ORDレコード
ord-5ab88f183228410d8e9d086ae1a6f981
出典データセット
uspto-grants-1994_04
特許番号
US05304556

反応ノート

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