Water → (9aS)-Octahydro-2H-pyrido[1,2-a]pyrazine

HRID 500443ノート

反応式

HRID 500443 の反応式
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

(S)-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 (S)-octahydro-2H-pyrido[1,2-a]pyrazine as a yellow oil (0.29 g, 2.07 mmol).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 0.5 h
  3. washThe filter cake was washed with tetrahydrofuran (2×5 ml)
  4. concentrationthe combined filtrate and washings concentrated

出典と根拠

ORDレコード
ord-5ad6a31487d34da289996b4d699885d7
出典データセット
uspto-grants-2010_08
特許番号
US07772227B2

反応ノート

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