4-Chloro-6-(phenylethynyl)pyrimidin-5-amine → 4-Chloro-6-phenyl-5H-pyrrolo[3,2-d]pyrimidine
반응식
[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:5]=[CH:4][N:3]=1>CN1C(=O)CCC1>[Cl:1][C:2]1[C:7]2[NH:8][C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[CH:9][C:6]=2[N:5]=[CH:4][N:3]=1참가 물질
3
실험 절차
To a solution of 251 (30.8 mg, 0.134 mmol) in NMP (1.4 mL) a suspension of KH in mineral oil (35%, 31 mL, 0.268 mmol) was added in one portion. The mixture was stirred at room temperature overnight and partitioned between EtOAc and water. The organic phase was collected, dried over anhydrous Na2SO4 and concentrated. The residue was purified by flash chromatography, eluent EtOAc/hexane (1:2) to afford title compound affording 252 (22.7 mg, 74% yield). MS (m/z): 230.1 (100%) 232.1 (33%) (M+1).
후처리
- additionwas added in one portion
- custompartitioned between EtOAc and water
- customThe organic phase was collected
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
- customThe residue was purified by flash chromatography, eluent EtOAc/hexane (1:2)
출처 및 근거
- ORD 기록
- ord-5c6928c172254802833c6f417e9a0e64
- 출처 데이터셋
- uspto-grants-2010_09
- 특허 번호
- US07790729B2
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