反応式
CN1C2C=CC=CC=2NC2N=CC=CC=2C1=O.[CH3:18][N:19]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[N:23]([CH2:30][CH2:31][O:32]C2CCCCO2)[C:22]2[N:39]=[CH:40][CH:41]=[CH:42][C:21]=2[C:20]1=[O:43].ClCCOC1CCCCO1>>[OH:32][CH2:31][CH2:30][N:23]1[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[N:19]([CH3:18])[C:20](=[O:43])[C:21]2[CH:42]=[CH:41][CH:40]=[N:39][C:22]1=2参加物
反応物 3
生成物 1
実験手順
Using a procedure analogous to that described in Example 2, 22.52 g (0.1 mol) of 6,11-dihydro-6-methyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one were convened to 6,11-dihydro-6-methyl-11-[2-[(2-tetrahydropyranyl)oxy]ethyl]-5H-pyrido-[2,3-b][1,5]benzodiazepin-5-one by reaction with 21.8 g (0.132 mol) of 1-chloro-2-[(2-tetrahydropyranyl)-oxy]-ethane. The raw material thus obtained was dissolved in a mixture of 500 ml ethanol and 100 ml of concentrated aqueous hydrochloric acid. After having been refluxed for two hours, the reaction mixture was evaporated in vacuo. The residue was triturated with ethanol, the precipitated crystals were faltered off and the solvent was removed from the filtrate by distillation in vacuo. The residue was purified by column chromatography on silica gel (0.2-0.5 mm) using chloroform/ethylacetate/methanol 5/5/1 (v/v/v) as an eluent. Colorless crystals of m.p. 133°-134° C. (after recrystallization from xylene) were obtained in a yield of 9.0 g (33% of theory).
出典と根拠
- ORDレコード
- ord-801c922ea1aa4db39b50a078b15ed6df
- 出典データセット
- uspto-grants-1996_11
- 特許番号
- US05571809
関連ノート
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