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C(OC(=O)[NH:7][C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=1[C:18]1[CH:23]=[C:22]([O:24][C:25]2[C:30]3[N:31]=[C:32]([NH:34][C:35](=[O:37])[CH3:36])[S:33][C:29]=3[CH:28]=[CH:27][CH:26]=2)[N:21]=[CH:20][N:19]=1)(C)(C)C.Cl>O1CCOCC1>[NH2:7][C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:15])[F:16])[CH:11]=[CH:10][C:9]=1[C:18]1[N:19]=[CH:20][N:21]=[C:22]([O:24][C:25]2[C:30]3[N:31]=[C:32]([NH:34][C:35](=[O:37])[CH3:36])[S:33][C:29]=3[CH:28]=[CH:27][CH:26]=2)[CH:23]=1참가 물질
4
실험 절차
To {2-[6-(2-acetylamino-benzothiazol-4-yloxy)-pyrimidin-4-yl]-5-trifluoromethyl-phenyl}carbamic acid tert-butyl ester, (Example 150) (0.35 g, 0.60 mmol) was added 4 M HCl in dioxane (25 mL). The mixture was stirred for 16 h and then was concentrated in vacuum. The residue was dissolved in ethyl acetate (40 mL) and washed with saturated NaHCO3 (2×70 mL), dried over Na2SO4 and concentrated in vacuum. Purification by silica gel chromatography (2:1, EtOAc:hexanes) afforded the title compound as thick yellow oil. Mp: 160–161° C. MS (ESI, pos. ion) m/z: 446 (M+1). Anal. Calcd for C20H14F3N5O2S.0.4H2O: C, 53.07; H, 3.30; F, 15.47; N, 12.59. Found: C, 53.12; H, 3.27; F, 15.19; N, 12.70.
후처리
- concentrationwas concentrated in vacuum
- dissolutionThe residue was dissolved in ethyl acetate (40 mL)
- washwashed with saturated NaHCO3 (2×70 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuum
- customPurification by silica gel chromatography (2:1, EtOAc:hexanes)
출처 및 근거
- ORD 기록
- ord-fef894ae32f5492ba620fd1981a988fe
- 출처 데이터셋
- uspto-grants-2006_12
- 특허 번호
- US07148221B2
연결된 노트
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