반응식
CN(C)C=O.CS([O:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:18])[F:17])(=O)=O.[Cl:20][C:21]1[C:25]([CH2:26][CH3:27])=[N:24][N:23]([CH3:28])[C:22]=1[C:29](O)=[O:30].C(=O)([O-])O.[Na+]>O>[Cl:20][C:21]1[C:25]([CH2:26][CH3:27])=[N:24][N:23]([CH3:28])[C:22]=1[C:29]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:18])[F:17])=[O:30]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 100 °C
실험 절차
To 10 ml of N,N-dimethylformamide were dissolved 0.50 g (2.2 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 0.45 g (2.4 mmol) of 4-chloro-5-ethyl-2-methyl-2H-pyrazole-3-carboxylic acid, followed by the addition of 0.37 g (4.4 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 7 hours. The reaction liquid was then poured in water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:19) to obtain 0.52 g (yield: 74%) of 6,6-difluoro-5-methyl-5-hexenyl 4-chloro-5-ethyl-2-methyl-2H-pyrazole-3-carboxylate.
후처리
- customThe reaction liquid
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
- customThe residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:19)
출처 및 근거
- ORD 기록
- ord-9bacae5831f746ef887ffa4a56025a9f
- 출처 데이터셋
- uspto-grants-2007_09
- 특허 번호
- US07273878B2
연결된 노트
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