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llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
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Water → HCID 9925691, Verbindung

HRID 1602877
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1602877
[H-].[Na+].[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.[CH2:11]([C:15]1[CH:20]=[C:19](Cl)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14].O>CN(C=O)C>[CH2:11]([C:15]1[CH:20]=[C:19]([O:3][CH2:4][C:5]2[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=2)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 114724-HydroxymethylpyridineHCID 24758Sodium hydrideHCID 15462308HCID 15462308, Verbindung

Produkt 1

HCID 9925691HCID 9925691, VerbindungAusbeute 42,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

60% sodium hydride, 0.55 g, was added to a 10 ml-solution of 1.6 g of 4-(hydroxymethyl)pyridine in DMF while being ice-cooled. After the mixture was stirred at 0° C. for 30 minutes, a DMF solution (2.5 ml) containing 2.6 g of 5-(3-butenyl)-7-chloropyrazolo[1,5-a]pyrimidine was added dropwise while being ice-cooled. The mixture was stirred at the same temperature for another 1 hour. After completion of the reaction, water was added to the reaction mixture. The crystals precipitated were collected by filtration and washed with water and then with diethyl ether. The crude crystals obtained were recrystallized from ethyl acetate-n-hexane to provide 1.5 g of the title compound as colorless crystals. The structure and melting point of the compound obtained are shown in Table 1.

Aufarbeitung

  1. temperaturecooled
  2. additionwas added dropwise
  3. temperaturecooled
  4. stirringThe mixture was stirred at the same temperature for another 1 hour
  5. additionwas added to the reaction mixture
  6. customThe crystals precipitated
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customThe crude crystals obtained
  10. customwere recrystallized from ethyl acetate-n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-4205bc1e009f4dff926864919b0a9bec
Quelldatensatz
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05985882

Notizen zur Reaktion

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