Hydrochloric Acid → 11-ethyl-5,11-dihydro-8-[2-(4-amino-2-methylphenoxy)ethyl]-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one
반응식
[CH2:1]([N:3]1[C:9]2[N:10]=[CH:11][C:12]([CH2:14][CH2:15][O:16][C:17]3[CH:22]=[CH:21][C:20]([NH:23]C(=O)OC(C)(C)C)=[CH:19][C:18]=3[CH3:31])=[CH:13][C:8]=2[C:7](=[O:32])[N:6]([CH3:33])[C:5]2[CH:34]=[CH:35][CH:36]=[N:37][C:4]1=2)[CH3:2].Cl.O1CCOCC1>>[CH2:1]([N:3]1[C:9]2[N:10]=[CH:11][C:12]([CH2:14][CH2:15][O:16][C:17]3[CH:22]=[CH:21][C:20]([NH2:23])=[CH:19][C:18]=3[CH3:31])=[CH:13][C:8]=2[C:7](=[O:32])[N:6]([CH3:33])[C:5]2[CH:34]=[CH:35][CH:36]=[N:37][C:4]1=2)[CH3:2]참가 물질
4
반응물 3
생성물 1
반응 조건
- 온도
- 25 °C
실험 절차
A mixture of 1,1-dimethylethyl N-{4-[2-(11-ethyl-6,11-dihydro-5-methyl-6-oxo-5H-dipyrido[3,2-b:2′,3′-e][1,4]diazepin-8-yl)ethoxy]-3-methylphenyl}carbamate (540 mg, 1.07 mmol) and 4 N HCl in 1,4-dioxane (5.0 mL, 20 mmol) was stirred at 25° C. for 2 h. The reaction mixture was concentrated under reduced pressure. The residue was taken in water (6 mL) and the resulting solution was washed with EtOAc. The aqueous layer was rendered basic (pH 9) with aqueous 2 N NaOH solution and the mixture was extracted with EtOAc. The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure to yield the title compound (398 mg, 92% yield) as a beige foam.
후처리
- concentrationThe reaction mixture was concentrated under reduced pressure
- washthe resulting solution was washed with EtOAc
- extractionthe mixture was extracted with EtOAc
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-c4aadd1f99a345b0bdb0ddb15aa4a63c
- 출처 데이터셋
- uspto-grants-2004_10
- 특허 번호
- US06806265B2
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