반응식
[NH2:1][C:2]1[C:11]([NH2:12])=[C:10]2[C:5]([C:6](=[O:23])[C:7]([C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)=[C:8]([CH:13]([CH3:15])[CH3:14])[O:9]2)=[CH:4][CH:3]=1.Cl.CCCCCC.C(OCC)C.[F:36][C:37]([F:42])([CH3:41])[C:38](O)=O>O>[Cl:22][C:19]1[CH:18]=[CH:17][C:16]([C:7]2[C:6](=[O:23])[C:5]3[CH:4]=[CH:3][C:2]4[NH:1][C:38]([C:37]([F:42])([F:36])[CH3:41])=[N:12][C:11]=4[C:10]=3[O:9][C:8]=2[CH:13]([CH3:14])[CH3:15])=[CH:21][CH:20]=1참가 물질
6
반응 조건
- 온도
- 110 °C
실험 절차
7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (168 mg, 0.511 mmol) is dissolved in 2,2-difluoropropionic acid (562 mg), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 110° C. for 4 h. The reaction mixture is cooled to room temperature, diluted with water (10 ml) and extracted with ethyl acetate (3×30 ml). The ethyl acetate extracts are combined and washed with saturated sodium bicarbonate solution (2×40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), treated with decolourising charcoal (50 mg), filtered and evaporated to give a colourless solid. This is sonicated with n-hexane/diethyl ether and filtered to give a cream-coloured powder.
후처리
- temperatureThe reaction mixture is cooled to room temperature
- extractionextracted with ethyl acetate (3×30 ml)
- washwashed with saturated sodium bicarbonate solution (2×40 ml) and saturated brine (40 ml)
- dry with materialThe organic layer is dried (MgSO4)
- additiontreated with decolourising charcoal (50 mg)
- filtrationfiltered
- customevaporated
- customto give a colourless solid
- filtrationfiltered
- customto give a cream-coloured powder
출처 및 근거
- ORD 기록
- ord-d6165b4813bc4d9eaebe17dccc6b897e
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07732435B2
연결된 노트
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