Ethanol → HCID 178487786, Verbindung

HRID 2073775

Reaktionsgleichung

Reaktionsgleichung von HRID 2073775
Cl[C:2]1[C:11]([C:12]#[N:13])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7](OC)[CH:8]=2)[N:3]=1.[OH2:16].[NH2:17][NH2:18].[CH2:19](O)C>>[CH3:19][O:16][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]1[NH:17][N:18]=[C:12]([NH2:13])[C:11]1=[CH:10]2

Komponenten

4

Edukt 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 8656122-Chloro-6-methoxyquinoline-3-carbonitrile

Produkt 1

HCID 178487786HCID 178487786, Verbindung

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a stirred suspension of 14.7 g 2-chloro-6-methoxy-3-quinolinecarbonitrile in 465 ml absolute ethanol was added 17 ml of hydrazine hydrate. The mixture was stirred at reflux for 24 hours and then cooled to 0° C. The resulting solid product was collected by filtration and boiled with 200 ml water to remove any hydrazine dihydrochloride present. The resulting material was filtered and dried in vacuo (90° C.), and recrystallized from 300 ml dimethylformamide to give 12.3 g 6-methoxy-1H-pyrazolo[3,4-b]quinolin-3-amine as a bright-yellow solid, m.p. >300° C.

Aufarbeitung

  1. temperatureat reflux for 24 hours
  2. filtrationThe resulting solid product was collected by filtration
  3. customto remove any hydrazine dihydrochloride present
  4. filtrationThe resulting material was filtered
  5. customdried in vacuo (90° C.)
  6. customrecrystallized from 300 ml dimethylformamide

Quellen und Nachweise

ORD-Eintrag
ord-e856b0b942ca4b188d232eb02f3ec0a3
Quelldatensatz
uspto-grants-1990_04
Patentnummer
US04920128

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