Water → HCID 12851825, Verbindung

HRID 1156898Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1156898
[C:1]1([CH3:19])[CH:6]=[CH:5][C:4]([C:7]([NH:9][CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=O)=[CH:3][CH:2]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O.[OH-].[Na+]>C1(C)C(C)=CC=CC=1.P(Cl)(Cl)(Cl)=O>[CH3:19][C:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:17]3[C:12](=[C:13]([Cl:18])[CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][N:9]=2)=[CH:3][CH:2]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 128518181-(p-Toluoylamino)-2-(2-chlorophenyl)ethane

Produkt 1

HCID 12851825HCID 12851825, VerbindungAusbeute 44,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7237O-XyleneLösungsmittelHCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

1-(p-Toluoylamino)-2-(2-chlorophenyl)ethane (70 g) was dissolved in 700 ml of xylene and 320 ml of phosphorus oxychloride, and while the solution was heated with stirring, 240 g of phosphorus pentoxide was added. The mixture was heated under reflux for 4 hours. Water was added to the reaction mixture. The aqueous layer was made weakly alkaline with an aqueous solution of sodium hydroxide, extracted with benzene, washed in water, and dried. The solvent was distilled off, and the residue was recrystallized from benzene to afford 29 g of 1-(4-methylphenyl)-5-chloro-3,4-dihydroisoquinoline as colorless needles.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. extractionextracted with benzene
  4. washwashed in water
  5. customdried
  6. distillationThe solvent was distilled off
  7. customthe residue was recrystallized from benzene

Quellen und Nachweise

ORD-Eintrag
ord-7719e64ba9a14481bd262f072a3001eb
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04337256

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