反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:29]=[CH:30][C:31]=1[F:32])[CH2:5][N:6]1[CH2:15][CH2:14][C:13]2[C:8](=[C:9]([OH:27])[C:10](=[O:26])[N:11]([CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH3:25])[C:12]=2[C:16]([O:18]C)=[O:17])[C:7]1=[O:28].[OH-].[K+].O1CCCC1CO.O>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:29]=[CH:30][C:31]=1[F:32])[CH2:5][N:6]1[CH2:15][CH2:14][C:13]2[C:8](=[C:9]([OH:27])[C:10](=[O:26])[N:11]([CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH3:25])[C:12]=2[C:16]([OH:18])=[O:17])[C:7]1=[O:28]参加物
4
反応物 3
生成物 1
反応条件
- 温度
- 50 °C
実験手順
Methyl 6-(3-chloro-4-fluorobenzyl)-4-hydroxy-2-[4-(methylamino)butyl]-3,5-dioxo-2,3,5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylate (0.18 g, 0.38 mmol) and potassium hydroxide (0.17 g, 2.3 mmol) in a mixture of 1:1:1 v/v/v tetrahydrofuran-methanol-water (4.5 mL) was heated at 50° C. overnight. The reaction mixture was concentrated under vacuum. The residue was partitioned between dichloromethane and dilute hydrochloric acid. The aqueous extract was concentrated under vacuum to provide the title compound as hydrochloride salt. This was used in the following step without further purification. ES MS M+1=452
後処理
- concentrationThe reaction mixture was concentrated under vacuum
- customThe residue was partitioned between dichloromethane and dilute hydrochloric acid
- extractionThe aqueous extract
- concentrationwas concentrated under vacuum
出典と根拠
- ORDレコード
- ord-edb76f37641c463b8fafa3e58110303d
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741315B2
関連ノート
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