反応式
O=[C:2]1[NH:7][CH2:6][C:5](=O)[N:4]2[CH2:9][CH2:10][CH2:11][CH2:12][C@H:3]12.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH2:2]1[NH:7][CH2:6][CH2:5][N:4]2[CH2:9][CH2:10][CH2:11][CH2:12][C@H:3]12参加物
6
反応条件
- 温度
- 0 °C
実験手順
(R)-Octahydro-1,4-dioxo-2H-pyrido[1,2-a]pyrazine (0.5 g, 2.98 mmol) was added portionwise to a stirred solution of lithium aluminium hydride (1M in tetrahydrofuran; 11.9 ml, 11.9 mmol). The resulting mixture was heated under reflux for 0.5 h. The solution was then cooled to 0° C. and treated dropwise with water (1.35 ml), 1 M sodium hydroxide solution (0.45 ml), then water (1.35 ml). Tetrahydrofuran (10 ml) was added and the solution stirred for 0.5 h, before filtration. The filter cake was washed with tetrahydrofuran (2×5 ml) and the combined filtrate and washings concentrated to yield (R)-octahydro-2H-pyrido[1,2-a]pyrazine as a yellow oil (0.29 g, 2.07 mmol).
後処理
- temperatureThe resulting mixture was heated
- temperatureunder reflux for 0.5 h
- washThe filter cake was washed with tetrahydrofuran (2×5 ml)
- concentrationthe combined filtrate and washings concentrated
出典と根拠
- ORDレコード
- ord-d8177b0d07644d80a3a48c4387a17559
- 出典データセット
- uspto-grants-2007_12
- 特許番号
- US07304064B2
関連ノート
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