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

HRID 500443Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 500443
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

Komponenten

6

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

(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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-5ad6a31487d34da289996b4d699885d7
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772227B2

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