Water → HCID 15733250, Verbindung

HRID 2397575Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2397575
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:16]=[CH:15][C:14]2[N:13]3[CH2:17][CH2:18][NH:19][C:20](=O)[C:12]3=[C:11]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:10]=2[CH:9]=1.O>O1CCCC1>[Cl:7][C:8]1[CH:16]=[CH:15][C:14]2[N:13]3[CH2:17][CH2:18][NH:19][CH2:20][C:12]3=[C:11]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:10]=2[CH:9]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 21436045HCID 21436045, Verbindung

Produkt 1

HCID 15733250HCID 15733250, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a stirred solution of lithium aluminum hydride (1 gram, 0.026 mole) in 20 ml dry tetrahydrofuran (THF) is added slowly a suspension of 1,2,3,4-tetrahydro-8-chloro-10-phenylpyrazino[1,2-a] indole-1-one (5.2 grams, 0.018 mole) in 40 ml of dry THF. This reaction mixture is stirred and refluxed for 8 hours after which it is cooled and decomposed by the slow addition of 3 ml of water. After stirring 1 hour the suspension is filtered. The filtercake is washed with isopropanol, THF, and acetone. The combined filtrate is taken to dryness and recrystallized from ethanol. The product is filtered off, washed with ether, and dried. The above titled product has a m.p. 163°-64° C. yield 4.5 grams (90%).

Aufarbeitung

  1. temperaturerefluxed for 8 hours after which it
  2. temperatureis cooled
  3. stirringAfter stirring 1 hour the suspension
  4. filtrationis filtered
  5. washThe filtercake is washed with isopropanol, THF, and acetone
  6. customrecrystallized from ethanol
  7. filtrationThe product is filtered off
  8. washwashed with ether
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b3a2bf8524284c32bd212dda3ff87acc
Quelldatensatz
uspto-grants-1977_05
Patentnummer
US04022778

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