Water → N-[2-bromo-4-[3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-(nitromethyl) butanoyl]phenylmethyl]phthalimide
반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8](=[O:23])[CH:9]=[C:10]([C:15]2[CH:20]=[C:19]([Cl:21])[CH:18]=[C:17]([Cl:22])[CH:16]=2)[C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][C:3]=1[CH2:24][N:25]1[C:29](=[O:30])[C:28]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]2[C:26]1=[O:35].[N+:36]([CH3:39])([O-:38])=[O:37].C1CCN2C(=NCCC2)CC1.O>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([C:8](=[O:23])[CH2:9][C:10]([C:15]2[CH:20]=[C:19]([Cl:21])[CH:18]=[C:17]([Cl:22])[CH:16]=2)([CH2:39][N+:36]([O-:38])=[O:37])[C:11]([F:14])([F:13])[F:12])[CH:5]=[CH:4][C:3]=1[CH2:24][N:25]1[C:26](=[O:35])[C:27]2=[CH:34][CH:33]=[CH:32][CH:31]=[C:28]2[C:29]1=[O:30]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
To a solution of 0.80 g of N-[2-bromo-4-[3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl]phenylmethyl]phthalimide and 0.12 g of nitromethane in 10 mL of acetonitrile, 0.23 g of 1,8-diazabicyclo[5,4,0]-7-undecene was added and the resultant reaction mixture was stirred at room temperature for 15 hours. After the completion of the reaction, 20 mL of water was added to the reaction mixture and the resultant reaction mixture was extracted with ethyl acetate (30 mL×2). The organic phase was dehydrated and dried over a saturated brine and anhydrous magnesium sulfate in this order and the solvent was distilled off under reduced pressure to obtain 0.90 g of the objective substance as a yellow resinoid.
후처리
- customthe resultant reaction mixture
- additionwas added to the reaction mixture
- customthe resultant reaction mixture
- extractionwas extracted with ethyl acetate (30 mL×2)
- dry with materialdried over a saturated brine and anhydrous magnesium sulfate in this order
- distillationthe solvent was distilled off under reduced pressure
- customto obtain 0.90 g of the objective substance as a yellow resinoid
출처 및 근거
- ORD 기록
- ord-0f872f93af16433980b6548412036ddd
- 출처 데이터셋
- uspto-grants-2012_09
- 특허 번호
- US08268754B2
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