반응식
[CH3:1][NH:2][CH:3]([C:5]1[CH:19]=[CH:18][C:8]2[N:9]([CH:12]3[CH2:17][CH2:16][CH2:15][CH2:14][O:13]3)[CH:10]=[N:11][C:7]=2[CH:6]=1)[CH3:4].Cl[C:21]1[N:26]=[C:25]([NH:27][C:28]2[NH:32][N:31]=[C:30]([CH:33]3[CH2:35][CH2:34]3)[CH:29]=2)[CH:24]=[CH:23][N:22]=1.CCN(C(C)C)C(C)C>CC(O)C>[CH:33]1([C:30]2[NH:31][N:32]=[C:28]([NH:27][C:25]3[CH:24]=[CH:23][N:22]=[C:21]([N:2]([CH3:1])[CH:3]([C:5]4[CH:19]=[CH:18][C:8]5[N:9]([CH:12]6[CH2:17][CH2:16][CH2:15][CH2:14][O:13]6)[CH:10]=[N:11][C:7]=5[CH:6]=4)[CH3:4])[N:26]=3)[CH:29]=2)[CH2:35][CH2:34]1참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 120 °C
실험 절차
A tube was charged with mixture of 84 (200 mg, 0.77 mmol), 53 (181 mg, 0.77 mmol) and DIPEA (200 mg, 1.5 mmol) in IPA (5 mL), sealed and stirred at 120° C. overnight. The reaction mixture was cooled to RT and concentrated under reduced pressure. The crude residue was purified by SiO2 chromatography eluting with a MeOH/DCM gradient (5% to 15% MeOH) to afford 68 mg (19%) of (±)-N4-(5-cyclopropyl-1H-pyrazol-3-yl)-N2-methyl-N2-(1-(1-(tetrahydro-2H-pyran-2-yl)-1H-benzo[d]imidazol-5-yl)ethyl)pyrimidine-2,4-diamine (86) as white solid: MS (ESI) m/z=459.2 (M+1).
후처리
- customsealed
- temperatureThe reaction mixture was cooled to RT
- concentrationconcentrated under reduced pressure
- customThe crude residue was purified by SiO2 chromatography
- washeluting with a MeOH/DCM gradient (5% to 15% MeOH)
출처 및 근거
- ORD 기록
- ord-509a0abd95fc485ebf44d9a342a30e85
- 출처 데이터셋
- uspto-grants-2014_01
- 특허 번호
- US08637537B2
연결된 노트
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