HCID 178448752, 화합물 → HCID 178520821, 화합물
반응식
C([N:5]1[C:9]([NH:10][C:11](=[O:19])[CH2:12][CH2:13][N:14]2[CH:18]=[CH:17][CH:16]=[N:15]2)=[CH:8][C:7]([C@@H:20]2[CH2:23][C@H:22]([O:24][C:25](=[O:34])[NH:26][CH2:27][CH:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)[CH2:21]2)=[N:6]1)(C)(C)C>C(O)(C(F)(F)F)=O>[N:14]1([CH2:13][CH2:12][C:11]([NH:10][C:9]2[NH:5][N:6]=[C:7]([C@@H:20]3[CH2:21][C@H:22]([O:24][C:25](=[O:34])[NH:26][CH2:27][CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)[CH2:23]3)[CH:8]=2)=[O:19])[CH:18]=[CH:17][CH:16]=[N:15]1참가 물질
3
실험 절차
A solution of cyclohexylmethyl-carbamic acid cis-3-[1-tert-butyl-5-(3-pyrazol-1-yl-propionylamino)-1H-pyrazol-3-yl]-cyclobutyl ester from Step A (122 mg) in TFA (2 mL) was heated at 120° C. in a microwave apparatus for 10 min. The solution was concentrated and the residue was dissolved in EtOAc. The resulting solution was washed sequentially with portions of saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution. The organic layer was dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography to afford the title product as a white solid. MS (M+H)+=415.5.
후처리
- concentrationThe solution was concentrated
- dissolutionthe residue was dissolved in EtOAc
- washThe resulting solution was washed sequentially with portions of saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated
- customThe residue was purified by silica gel chromatography
출처 및 근거
- ORD 기록
- ord-750775f380f14ffd8839029ab170e442
- 출처 데이터셋
- uspto-grants-2010_03
- 특허 번호
- US07671072B2
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