Phosphorus oxide (P4O10) → HCID 12851821, Verbindung

HRID 1156868Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1156868
[Br:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]([NH:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])=O)=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]2[C:16]3[C:11](=[C:12]([CH3:17])[CH:13]=[CH:14][CH:15]=3)[CH2:10][CH2:9][N:8]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 14812Phosphorus oxide (P4O10)HCID 24813Phosphorus oxychlorideHCID 128518091-(4-Bromobenzoylamino)-2-(2-methylphenyl)ethane

Produkt 1

HCID 12851821HCID 12851821, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

Forty-four (44) grams of 1-(4-bromobenzoylamino)-2-(2-methylphenyl)ethane was heated with stirring at 140° C. for 4 hours together with 300 ml of xylene, 100 ml of phosphorus oxychloride and 100 g of phosphorus pentoxide. The reaction mixture was decanted to remove the solvent. The residue was carefully decomposed with ice water, and made weakly alkaline with an aqueous solution of sodium hydroxide. The crystals precipitated were extracted with benzene, and dried, followed by distilling off the solvent. Recrystallization of the residue from hexane afforded 35 g of 1-(4-bromophenyl)-5-methyl-3,4-dihydroisoquinoline as colorless needles having a melting point of 60.0° to 61.5° C.

Aufarbeitung

  1. customThe reaction mixture was decanted
  2. customto remove the solvent
  3. customThe crystals precipitated
  4. extractionwere extracted with benzene
  5. customdried
  6. distillationby distilling off the solvent
  7. customRecrystallization of the residue from hexane

Quellen und Nachweise

ORD-Eintrag
ord-4a5359cb006448359935601ed1a06d2b
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04337256

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