Water → HCID 15230482, 화합물

HRID 1464294노트

반응식

HRID 1464294 반응식
[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

참가 물질

7

반응물 4

HCID 962WaterHCID 7815p-ChlorothiophenolHCID 24758Sodium hydrideHCID 869878HCID 869878, 화합물

생성물 1

HCID 15230482HCID 15230482, 화합물수율 50.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ab88f183228410d8e9d086ae1a6f981
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05304556

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