반응식
[CH2:1](Cl)[CH2:2]Cl.[CH:5]([N:8](C(C)C)CC)(C)[CH3:6].C(N)C1C=CC=CC=1.C(OC(N1CCCC1[C:34](=O)[NH:35][C:36]1[CH:41]=C(Cl)[CH:39]=[CH:38][C:37]=1[C:43](=[O:52])[NH:44][CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)=O)(C)(C)C.Cl[CH2:55][Cl:56]>>[CH2:45]([N:44]1[C:43](=[O:52])[C:37]2[C:36](=[CH:41][C:55]([Cl:56])=[CH:39][CH:38]=2)[N:35]([CH:2]2[CH2:1][CH2:6][CH2:5][NH:8]2)[CH2:34]1)[C:46]1[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=1참가 물질
반응물 5
생성물 1
실험 절차
To a solution of the compound of Formula 104 (8.7 9, 24 mmol) in dichloromethane (250 mL) was added EDC (14.85 g, 77 mmol), and diisopropylethylamine (14.1 mL, 81 mmol). After stirring at room temperature for 1.5 hours, benzylamine (8.4 mL, 77 mmol) was added and the reaction stirred for an additional 48 hours. The mixture was washed with water (2×50 mL), 10% phosphoric acid (2×50 mL), and saturated NaHCO3 (50 mL). The organic phase was dried over MgSO4, filtered and concentrated under vacuum to give a mixture of 9.4 g (88% yield) of the desired product of Formula 105, 2-(2-benzylcarbamoyl-5-chloro-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester, as a light yellow foam, together with a small amount of 2-(3-benzyl-7-chloro-4-oxo-3,4-dihydro-2Hquinzoline-1-yl)-pyrrolidine-1-carboxylic acid tert-butyl ester (Formula 106), which was taken on without further purification. LRMS (MH+) m/z 458.
후처리
- stirringthe reaction stirred for an additional 48 hours
- washThe mixture was washed with water (2×50 mL), 10% phosphoric acid (2×50 mL), and saturated NaHCO3 (50 mL)
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated under vacuum
- customto give
출처 및 근거
- ORD 기록
- ord-924983f59a61409b9a502dc7aa2b72b5
- 출처 데이터셋
- uspto-grants-2009_07
- 특허 번호
- US07557115B2
연결된 노트
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