Ethanol → HCID 54461106, Verbindung

HRID 616722Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 616722
[C:1]1([C:7]2[C:19]([C:20]([OH:22])=[O:21])=[C:10]3[C:11]4[C:16]([CH2:17][CH2:18][N:9]3[N:8]=2)=[CH:15][CH:14]=[CH:13][CH:12]=4)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)Cl.C(=O)(O)[O-].[Na+].[CH2:32](O)[CH3:33]>>[CH2:32]([O:21][C:20]([C:19]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][N:9]2[CH2:18][CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]=12)=[O:22])[CH3:33]

Komponenten

5

Edukt 4

HCID 702EthanolHCID 24386Thionyl Chloride2×HCID 516892Sodium BicarbonateHCID 12948308HCID 12948308, Verbindung

Produkt 1

HCID 54461106HCID 54461106, Verbindung

Versuchsvorschrift

2-Phenyl-5,6-dihydro-pyrazolo[5,1-a]isoquinoline-1-carboxylic acid (7.48 g.) is stirred at 90° C. for three hours with 3.77 ml. of SOCl2. The thionyl chloride excess is eliminated in vacuo and the residual acid chloride is dissolved in 80 ml. of ethanol at 40°-50° C. After 15 minutes, the reaction mixture is neutralized by addition of aqueous sodium bicarbonate and the solvent is eliminated by distillation. The residue is extracted with ethyl ether and, after evaporation of the organic solution, is crystallized from isopropyl ether. Yield of title compound 2.47 g.; m.p. 84°-5° C.

Aufarbeitung

  1. customat 40°-50° C
  2. distillationthe solvent is eliminated by distillation
  3. extractionThe residue is extracted with ethyl ether
  4. customafter evaporation of the organic solution
  5. customis crystallized from isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-320aeeb2af37423dbca0ebc841aa7c77
Quelldatensatz
uspto-grants-1978_02
Patentnummer
US04075342

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