반응식
CCN(C(C)C)C(C)C.[CH2:10]([O:17][C:18]1[CH:32]=[CH:31][C:21]([C:22]([NH:24][C:25]([CH3:30])([CH3:29])[C:26]([OH:28])=O)=[O:23])=[CH:20][CH:19]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[N:55]1([C:61]([C:63]2[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=2[C:69]([F:72])([F:71])[F:70])=[O:62])[CH2:60][CH2:59][NH:58][CH2:57][CH2:56]1>CN(C=O)C.O>[CH2:10]([O:17][C:18]1[CH:19]=[CH:20][C:21]([C:22]([NH:24][C:25]([CH3:30])([CH3:29])[C:26](=[O:28])[N:58]2[CH2:59][CH2:60][N:55]([C:61](=[O:62])[C:63]3[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=3[C:69]([F:72])([F:70])[F:71])[CH2:56][CH2:57]2)=[O:23])=[CH:31][CH:32]=1)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1참가 물질
반응물 5
생성물 1
시약·촉매·용매 2
실험 절차
DIPEA (284 mg, 0.19 mL, 1.62 mmol) was added to a stirred solution of 2-(4-benzyloxy-benzoylamino)-2-methyl-propionic acid (170 mg, 0.54 mmol) in DMF (2 mL). HOBT (88 mg, 0.65 mmol) and EDCI (125 mg, 0.65 mmol) were then added at room temperature. After 2 minutes, piperazin-1-yl-(2-trifluoromethyl-phenyl)-methanone hydrochloride salt (192 mg, 0.65 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and filtered the solid precipitated out to afford 150 mg (50% yield) of 4-benzyloxy-N-{1,1-dimethyl-2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide. LCMS Purity: 93.29%. 1H NMR (DMSO-d6): δ 8.4 (bs, 1H), 7.6-7.8 (m, 5H), 7.4 (m, 6H), 7.0-7.1 (d, 2H), 5.2 (m, 2H), 3.5 (m, 5H), 3.0 (m, 3H), 1.4 (s, 6H).
후처리
- filtrationfiltered the solid
- customprecipitated out
출처 및 근거
- ORD 기록
- ord-70f54ed9e03b4e659104debb51e72d80
- 출처 데이터셋
- uspto-grants-2010_11
- 특허 번호
- US07842696B2
연결된 노트
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