Dimethylformamide → 4-{[(2-{1-[5-(4-tert-butylphenyl)-1-benzyl-4-hydroxy-1H-pyrazol-3-yl]ethylidene}hydrazino)carbonothioyl]amino}benzoic acid

HRID 2103827노트

반응식

HRID 2103827 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:15]([CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:14]=[C:13]([C:23](=O)[CH3:24])[C:12]=2[OH:26])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[NH:27]([C:29]([NH:31][C:32]1[CH:40]=[CH:39][C:35]([C:36]([OH:38])=[O:37])=[CH:34][CH:33]=1)=[S:30])[NH2:28].CN(C)C=O>Cl.O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:15]([CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:14]=[C:13]([C:23](=[N:28][NH:27][C:29]([NH:31][C:32]3[CH:40]=[CH:39][C:35]([C:36]([OH:38])=[O:37])=[CH:34][CH:33]=3)=[S:30])[CH3:24])[C:12]=2[OH:26])=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 3

HCID 6228DimethylformamideHCID 27573784-(4-Carboxyphenyl)-3-thiosemicarbazideHCID 670500891-[5-(4-tert-butylphenyl)-1-benzyl-4-hydroxy-1H-pyrazol-3-yl]ethanone

생성물 1

HCID 723599354-{[(2-{1-[5-(4-tert-butylphenyl)-1-benzyl-4-hydroxy-1H-pyrazol-3-yl]ethylidene}hydrazino)carbonothioyl]amino}benzoic acid수율 70.3%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 962Water용매

실험 절차

1-[5-(4-tert-Butylphenyl)-1-benzyl-4-hydroxy-1H-pyrazol-3-yl]ethanone (0.218 mmol, 76 mg) and 4-hydrazinocarbonothioylaminobenzoic acid (0.218 mmol, 46 mg) were stirred with dimethylformamide (3.5 mL) and three drops of concentrated hydrochloric acid at room temperature for 22 hours. After addition of water, the precipitated yellow solid was recovered by filtration, washed with water and dried by means of a vacuum pump. The resulting solid was stirred with chloroform/n-hexane for a while, then recovered by filtration and dried by means of a vacuum pump to give the desired product as a pale yellow solid (83 mg, yield 70%).

후처리

  1. filtrationthe precipitated yellow solid was recovered by filtration
  2. washwashed with water
  3. customdried by means of a vacuum pump
  4. filtrationrecovered by filtration
  5. customdried by means of a vacuum pump

출처 및 근거

ORD 기록
ord-493797eec8cd4b7c837eaa617156e9ef
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576115B2

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