反応式
[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([CH:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[CH2:11][C@@H:10]([NH:25]C(OC(C)(C)C)=O)[C:9]1=[O:33])=[O:6])([CH3:4])([CH3:3])[CH3:2].Cl.O.C(OCC)C>C(O)C>[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([CH:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[CH2:11][C@@H:10]([NH2:25])[C:9]1=[O:33])=[O:6])([CH3:4])([CH3:2])[CH3:3]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 60 °C
実験手順
To a solution of 63.5 g of (R)-1-tert-butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine in 100 ml of ethanol was added 100 ml of 6N hydrochloric acid. The mixture was stirred at 60° C. for 1.5 hours. After the reaction mixture was cooled to room temperature, a mixed solvent of water and diethyl ether (1:1) was added. The aqueous layer was separated, neutralized with a 6N aqueous solution of sodium hydroxide, and then extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate and evaporated under reduced pressure, whereby 46.3 g of (R)-(−)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine was obtained.
後処理
- temperatureAfter the reaction mixture was cooled to room temperature
- customThe aqueous layer was separated
- extractionextracted with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-d3610f679fbf416bbd60b2c9044db414
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06747022B2
関連ノート
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