反応式
[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]=1参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 0 °C
実験手順
(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+).
後処理
- 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
出典と根拠
- ORDレコード
- ord-8da343e23cc24acd828e859b0586d42e
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425551B2
関連ノート
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