반응식
[H-].[Na+].[CH2:3]([C:5]1([CH2:20][CH3:21])[C:11](=[O:12])[NH:10][C:9]2[CH:13]=[CH:14][C:15]([O:17][CH3:18])=[CH:16]C=2NC1=O)[CH3:4].[CH3:22]I.O.[CH3:25][N:26]([CH:28]=[O:29])[CH3:27]>C(OCC)(=O)C>[CH2:20]([C:5]1([CH2:3][CH3:4])[C:11](=[O:12])[N:10]([CH3:22])[C:9]2[CH:13]=[CH:14][C:15]([O:17][CH3:18])=[CH:16][C:25]=2[N:26]([CH3:27])[C:28]1=[O:29])[CH3:21]참가 물질
반응물 5
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 0 °C
실험 절차
Sodium hydride (60% in oil, 170 mg, 4.3 mmol) was suspended in DMF (15 ml). 3,3-Diethyl-7-methoxy-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (452 mg, 1.7 mmol) was added thereto at 0° C., and stirring was conducted at the same temperature for 1 hour. Methyl iodide (0.42 ml, 6.8 mmol) was added to the mixture, and stirred at room temperature for 3 days. Water was added to the reaction mixture and extraction with ethyl acetate was performed. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1→1:1). The purified product was concentrated to dryness under reduced pressure to thereby obtain 373 mg (yield: 76%) of 3,3-diethyl-7-methoxy-1,5-dimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione as a white powder.
후처리
- stirringstirred at room temperature for 3 days
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1→1:1)
- concentrationThe purified product was concentrated to dryness under reduced pressure
출처 및 근거
- ORD 기록
- ord-23ff7ecae9684bd4a4b1d8e389494ada
- 출처 데이터셋
- uspto-grants-2012_12
- 특허 번호
- US08338406B2
연결된 노트
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