1-Isoquinolinamine → STK019752

HRID 1680628Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1680628
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[C:12]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:17]=[CH:16][C:15]([CH:18]([C:20](C(Br)C2C=CC(C3C=CC=CC=3)=CC=2)=O)Br)=[CH:14][CH:13]=1>C(Cl)(Cl)Cl>[C:12]1([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:13]=[CH:14][C:15]([C:18]2[N:1]=[C:2]3[C:11]4[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=4)[CH:5]=[CH:4][N:3]3[CH:20]=2)=[CH:16][CH:17]=1

Komponenten

4

Edukt 2

HCID 737421-IsoquinolinamineHCID 86737811HCID 86737811, Verbindung

Produkt 1

HCID 1338745STK019752

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A solution of 4.32 g. (0.03 mole) of 1-amino-isoquinoline and 8.25 g. (0.03 mole) of [(1,1'-biphenyl)-4-yl]-bromomethyl-ketone in 100 ml. of chloroform was heated on a boiling water bath for about 10 minutes until a precipitate separated. The solvent was distilled off at atmospheric pressure and the residue was heated under vacuum for 30 minutes at 100° C. It was subsequently taken up with 50 ml of water and the resulting solution was made alkaline by means of 70 ml. of aqueous 10% sodium hydroxide. After extracting with 500 ml. of methylene chloride and evaporating the solvent, a residue was obtained which was re-crystallized from ethylene glycol monomethylether. Yield 3.0 g. M.p. 221°-22° C.

Aufarbeitung

  1. customseparated
  2. distillationThe solvent was distilled off at atmospheric pressure
  3. extractionAfter extracting with 500 ml
  4. customof methylene chloride and evaporating the solvent
  5. customa residue was obtained which
  6. customwas re-crystallized from ethylene glycol monomethylether

Quellen und Nachweise

ORD-Eintrag
ord-f383a06c7a864e16859ea63dff939c2c
Quelldatensatz
uspto-grants-1981_06
Patentnummer
US04275066

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