Ethyl Acetate → 5-Bromo-2-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methyl-N-(pyrrolidin-1-yl)pyrimidin-4-amine
반응식
[Br:1][C:2]1[C:3]([NH:16][NH2:17])=[N:4][C:5]([N:9]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]2[CH3:15])=[N:6][C:7]=1[CH3:8].[CH3:18][C:19](N(C)C)=O.[CH3:24][CH2:25]OC(C)=O>>[Br:1][C:2]1[C:3]([NH:16][N:17]2[CH2:18][CH2:19][CH2:25][CH2:24]2)=[N:4][C:5]([N:9]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]2[CH3:15])=[N:6][C:7]=1[CH3:8]참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
To a flask was added 1-(5-bromo-2-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methylpyrimidin-4-yl)hydrazine (100 mg, 0.34 mmol) 1,4-dibromobutane (0.04 ml, 0.37 mmol) hunig's base (0.18 ml, 1.01 mmol) and DMAC (1.0 ml) at R.T. After heating at 60° C. over night, the reaction mixture was cooled to R.T. and diluted with EtOAc (2 ml) the white solid was filtered and the mother liquor was concentrated under reduced pressure. The resulting residue was purified by column chromatography eluted with 30% EtOAc:hex to give the titled compound weighted 76 mg 64%
후처리
- temperaturethe reaction mixture was cooled to R.T.
- filtrationwas filtered
- concentrationthe mother liquor was concentrated under reduced pressure
- customThe resulting residue was purified by column chromatography
- washeluted with 30% EtOAc
출처 및 근거
- ORD 기록
- ord-07381ae7b8e64c82b3eb2c104e3f2d70
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07696213B2
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