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Ammonia → HCID 19707339, Verbindung

HRID 1379076
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1379076
[C:1]1([CH2:7][C:8](O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:11][NH2:12].N.[CH2:14]1[CH:23]2[CH:18]([CH2:19][CH2:20][C:21]3[CH:27]=[CH:26][CH:25]=[CH:24][C:22]=32)[NH:17][C:16](=[O:28])[CH2:15]1>C(O)CO.COCCOCCOC>[CH3:11][N:17]1[C:18]2[C:7]([CH3:8])([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][C:6]=3[CH2:22][CH:23]=2)[CH2:14][CH2:15][C:16]1=[O:28].[CH3:11][N:12]1[C@@H:18]2[C@:23]([CH3:1])([C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[CH2:20][CH2:19]2)[CH2:14][CH2:15][C:16]1=[O:28]
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Komponenten

8

Edukt 4

HCID 222AmmoniaHCID 999Phenylacetic AcidHCID 6329MethylamineHCID 19707357HCID 19707357, Verbindung

Produkt 2

HCID 19707339HCID 19707339, VerbindungHCID 53780108HCID 53780108, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 174Ethylene GlycolLösungsmittel
HCID 8150DiglymeLösungsmittel

Versuchsvorschrift

By following the procedures described in Example 40, Steps A, B, C, D, E and F using phenylacetic acid as the starting material and in Step F using methylamine rather than ammonia and diglyme rather than ethylene glycol, the compound 4-methyl-10b-methyl-1,2,3,4,6,10b-hexahydrobenzo[f]quinolin-3-one was prepared. This hexahydrobenzo[f]quinolin-3-one was hydrogenated by following the procedures described in Example 22 except that the reaction was carried out at 60° C. over 7 hours. The reaction mixture was filtered and solvent evaporated under vacuum. The residue was purified by chromatography on SiO2 (CHCl3 as eluent) followed by recrystallization from ethyl acetate/hexanes to afford 154 mg of the title compound. Melting point 111°-113° C.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customsolvent evaporated under vacuum
  3. customThe residue was purified by chromatography on SiO2 (CHCl3 as eluent)
  4. customfollowed by recrystallization from ethyl acetate/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-ef8ca90095874a29ab06f5a317b20aab
Quelldatensatz
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05670512

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