4-Acetylaminopyrazole → HCID 20561808, 화합물
반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](=[O:15])[CH:13](Br)[C:12]([NH:17][C:18](=[O:48])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([NH:25][C:26](=[O:47])[CH:27]([O:30][C:31]3[CH:36]=[CH:35][C:34]([C:37]([CH2:40][CH3:41])([CH3:39])[CH3:38])=[CH:33][C:32]=3[C:42]([CH2:45][CH3:46])([CH3:44])[CH3:43])[CH2:28][CH3:29])[CH:20]=2)=[N:11]1.[C:49]([NH:52][C:53]1[CH:54]=[N:55][NH:56][CH:57]=1)(=[O:51])[CH3:50]>C(OCC)(=O)C>[C:49]([NH:52][C:53]1[CH:54]=[N:55][N:56]([CH:13]2[C:14](=[O:15])[N:10]([C:3]3[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=3[Cl:9])[N:11]=[C:12]2[NH:17][C:18](=[O:48])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([NH:25][C:26](=[O:47])[CH:27]([O:30][C:31]3[CH:36]=[CH:35][C:34]([C:37]([CH2:40][CH3:41])([CH3:39])[CH3:38])=[CH:33][C:32]=3[C:42]([CH2:45][CH3:46])([CH3:44])[CH3:43])[CH2:28][CH3:29])[CH:20]=2)[CH:57]=1)(=[O:51])[CH3:50]참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
17.8 g of 1-(2,4,6-trichlorophenyl)-3-{3-[2-(2,4-di-tert-amylphenoxy)butyramido]benzamido}-4-bromo-5-oxo-2-pyrazoline and 10 g of 4-acetamidopyrazole were well mixed in a mortar and heated at 100° C. for 2 hours. To the reaction mixture, 200 cc of ethyl acetate was added and the mixture was washed several times with water. The ethyl acetate layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from a solvent mixture of acetonitrile and ethyl acetate, 12.1 g of Coupler (1) was obtained. The melting point of the coupler was 135° to 141° C.
후처리
- washthe mixture was washed several times with water
- dry with materialThe ethyl acetate layer was dried with anhydrous sodium sulfate
- concentrationconcentrated
- customUpon crystallization of the residue
- additionfrom a solvent mixture of acetonitrile and ethyl acetate, 12.1 g of Coupler (1)
- customwas obtained
- customwas 135° to 141° C.
출처 및 근거
- ORD 기록
- ord-e03b12032fce4a3884916c517b2facce
- 출처 데이터셋
- uspto-grants-1981_11
- 특허 번호
- US04301235
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