반응식
[CH3:1][C:2]1([CH3:12])[C:10]2[C:5](=[C:6]([NH2:11])[CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.N1C=CC=CC=1.[Cl:19][C:20]1[N:24]([CH3:25])[N:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[C:21]=1[C:30](Cl)=[O:31].O>C1(C)C=CC=CC=1>[Cl:19][C:20]1[N:24]([CH3:25])[N:23]=[C:22]([C:26]([F:28])([F:27])[F:29])[C:21]=1[C:30]([NH:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH2:4][CH2:3][C:2]2([CH3:12])[CH3:1])=[O:31]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
To a solution of 1.61 g of 1,1-dimethyl-4-aminoindane and 2 ml of pyridine in 50 ml of toluene was added drop by drop with stirring at room temperature a solution of 2.47 g of 5-chloro-1-methyl-3-trifluoromethylpyrazole-4-carboxylic acid chloride in 10 ml of toluene, followed by stirring at room temperature for 12 hours. Thereafter, the reaction solution was poured into a cold water to result in separation into two layers. The aqueous layer was extracted with ethyl acetate. The resultant organic layer was dried over anhydrous magnesium sulfate and the soluent was distilled off. The residue was recrystallized using toluene to obtain 3.01 g of 5-chloro-1-methyl-3-trifluoromethyl-N-(1,1-dimethylindane-4-yl)pyrazole-4-carboxamide having a melting point of 119.9° C.
후처리
- customto result in separation into two layers
- extractionThe aqueous layer was extracted with ethyl acetate
- dry with materialThe resultant organic layer was dried over anhydrous magnesium sulfate
- distillationthe soluent was distilled off
- customThe residue was recrystallized
출처 및 근거
- ORD 기록
- ord-a8d03a69425d4a02b93aee7f9c20ed2b
- 출처 데이터셋
- uspto-grants-1988_05
- 특허 번호
- US04742074
연결된 노트
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