반응식
[NH2:1][C@@H:2]1[C:8](=[O:9])[N:7]([CH2:10][CH2:11][O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:6]2[CH:20]=[CH:21][CH:22]=[CH:23][C:5]=2[C:4]2[CH:24]=[CH:25][CH:26]=[CH:27][C:3]1=2.[C:28](O)(=[O:32])[C@H:29]([CH3:31])[OH:30].ON1C2C=CC=CC=2N=N1.C(Cl)CCl>C1COCC1.O.C(OCC)(=O)C>[CH2:13]([O:12][CH2:11][CH2:10][N:7]1[C:8](=[O:9])[C@@H:2]([NH:1][C:28](=[O:32])[C@@H:29]([OH:30])[CH3:31])[C:3]2[CH:27]=[CH:26][CH:25]=[CH:24][C:4]=2[C:5]2[CH:23]=[CH:22][CH:21]=[CH:20][C:6]1=2)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1참가 물질
8
반응물 4
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 0 °C
실험 절차
(S)-7-Amino-5-(2-benzyloxy-ethyl)-5H,7H-dibenzo[b,d]azepin-6-one (50 mg, 0.14 mmol) and L-(+)-lactic acid (14 mg, 0.15 mmol) were dissolved in THF (2 ml), cooled to 0° C. and under exclusion of moisture subsequently treated with 1-hydroxybenzotriazole (21 mg, 0.15 mmol), EDC (33 mg, 0.17 mmol) and N-diisopropyl-ethylamine (0.05 ml, 0.28 mmol). After stirring for 30 min. at 0° C. and 3 h at ambient temperature, the mixture was diluted with water and ethyl acetate (10 ml each), the phases separated and the organic layer extracted with water, 1N aqueous HCl and saturated aqueous NaCl. After drying over magnesium sulphate and evaporation of the solvent, the title compound was afforded as colourless oil (98%). MS: m/e=431(M−H+).
후처리
- customthe phases separated
- extractionthe organic layer extracted with water, 1N aqueous HCl and saturated aqueous NaCl
- dry with materialAfter drying over magnesium sulphate and evaporation of the solvent
출처 및 근거
- ORD 기록
- ord-8da343e23cc24acd828e859b0586d42e
- 출처 데이터셋
- uspto-grants-2008_09
- 특허 번호
- US07425551B2
연결된 노트
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