Iodoethane → L 11204

HRID 616692Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 616692
[OH:1][C:2]1[CH:3]=[C:4]([C:8]2[N:20]=[C:11]3[C:12]4[C:17]([CH2:18][CH2:19][N:10]3[N:9]=2)=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:5]=[CH:6][CH:7]=1.[O-][CH2:22][CH3:23].[Na+].C(I)C>C(O)C>[CH2:22]([O:1][C:2]1[CH:3]=[C:4]([C:8]2[N:20]=[C:11]3[C:12]4[C:17]([CH2:18][CH2:19][N:10]3[N:9]=2)=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:5]=[CH:6][CH:7]=1)[CH3:23]

Komponenten

5

Edukt 3

HCID 6340Iodoethane2×HCID 134401m-(5,6-Dihydro-s-triazolo(5,1-a)isoquinolin-2-yl)phenolHCID 2723922Sodium ethoxide

Produkt 1

HCID 119282L 11204

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

2-(3-Hydroxyphenyl)-5,6-dihydro-s-triazolo-[5,1-a]isoquinoline (3.95 g.) is added to 60 ml. of ethanol containing one equivalent proportion of sodium ethoxide. To this mixture is added 1.57 ml. of ethyl iodide in 15 ml. of ethanol. After stirring for one hour at room temperature, a further 1.57 ml. of ethyl iodide is added and the mixture is refluxed for 18 hours. The solvent is distilled off and the residue is washed with water and extracted with dichloromethane. Evaporation of the solvent and crystallization of the residue from ethanol gives 3.87 g. of the title product; m.p. 102°-3° C.

Aufarbeitung

  1. additionTo this mixture is added 1.57 ml
  2. temperaturethe mixture is refluxed for 18 hours
  3. distillationThe solvent is distilled off
  4. washthe residue is washed with water
  5. extractionextracted with dichloromethane
  6. customEvaporation of the solvent and crystallization of the residue from ethanol
  7. customgives 3.87 g

Quellen und Nachweise

ORD-Eintrag
ord-7eb89bf05afa4e17aa7912120d86889f
Quelldatensatz
uspto-grants-1978_02
Patentnummer
US04075341

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