Potassium Hydroxide → Ihch-7113

HRID 629316Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 629316
[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]3[C@@H:12]4[CH2:17][N:16](C(OCC)=O)[CH2:15][CH2:14][C@@H:13]4[N:5]([C:6]=23)[CH2:4][CH2:3]1.[OH-].[K+]>C(O)CCC>[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]3[C@@H:12]4[CH2:17][NH:16][CH2:15][CH2:14][C@@H:13]4[N:5]([C:6]=23)[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 21302624Ethyl (6bR,10aS)-2,3,6b,9,10,10a-hexahydro-3-methyl-1H-pyrido(3',4':4,5)pyrrolo(1,2,3-de)quinoxaline-8(7H)-carboxylate

Produkt 1

HCID 21302499Ihch-7113

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

Ethyl(6bR,10aS)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H-pyrido-[3′,4′:4,5]-pyrrolo[1,2,3-de]quinoxaline-8-carboxylate (ca. 18.5 g, 57 mmol), KOH (12.7 g, 226 mmol) and n-butanol are placed in a 300 ml pressure bottle and heated in an oil bath at 120° C. for 3 hours. n-butanol is removed in vacuo and 300 ml of water is added and then extracted with DCM. The DCM layers are combined and washed with brine and dried (Na2SO4). Evaporation of the solvent gives (6bR,10aS)-3-methyl-2,3,6b,7,8,9,10,10a-octahydro-1H-pyrido-[3′,4′:4,5]-pyrrolo[1,2,3-de]quinoxaline.

Aufarbeitung

  1. customn-butanol is removed in vacuo and 300 ml of water
  2. additionis added
  3. extractionextracted with DCM
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. customEvaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-3d3db8fb8b484203bad9ba6b642095cd
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315504B2

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