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
反応式
[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]参加物
4
反応物 3
生成物 1
反応条件
- 温度
- 25 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-c4aadd1f99a345b0bdb0ddb15aa4a63c
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06806265B2
反応ノート
読み込み中…