반응식
[CH3:1][O:2][C:3](=[O:9])[C@H:4]([CH:6]([CH3:8])[CH3:7])[NH2:5].CN1CCOCC1.CCN=C=NCCCN(C)C.Cl.[C:29](O)(=[O:36])[C:30]1[CH:35]=[CH:34][CH:33]=[N:32][CH:31]=1>C(Cl)Cl.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:9])[C:4]([NH2:5])([C:29]([C:30]1[CH:31]=[N:32][CH:33]=[CH:34][CH:35]=1)=[O:36])[CH:6]([CH3:8])[CH3:7]참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 25 °C
실험 절차
To a solution of L-valine methylester (3.0 g, 2.29 mmol), in DCM (30 mL) were added N-methyl morpholine (11.5 mL, 11.45 mmol), EDCI.HCl (8.7 g, 45.8 mmol) and nicotinic acid (3.3 g, 27.4 mmol). The mixture was allowed to stir at room temperature (25° C.) over 3 h under nitrogen atmosphere. The resulting mixture was diluted with ethyl acetate (200 mL), washed with water (3×100mL) and dried over sodium sulphate. The crude product obtained upon evaporation of the solvent was further purified by silica gel column chromatography to obtain required product as sticky solid (2.0 g, 38%).
후처리
- washwashed with water (3×100mL)
- dry with materialdried over sodium sulphate
- customThe crude product obtained upon evaporation of the solvent
- customwas further purified by silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-c149b7e51eb84d4c872955058ddfdce3
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846721B2
연결된 노트
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