Ethanol → 1H-Indazole-1-propanamine, 3-amino-N,N-diethyl-

HRID 580119Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 580119
C(O)C.[CH2:4]([N:6]([CH2:30][CH3:31])[CH2:7][CH2:8][CH2:9][N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([N:19]2C(=O)C3=CC=CC=C3C2=O)=[N:11]1)[CH3:5].O.NN>O>[CH2:30]([N:6]([CH2:4][CH3:5])[CH2:7][CH2:8][CH2:9][N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([NH2:19])=[N:11]1)[CH3:31]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 201358851-(3-Diethylaminopropyl)-3-phthalimidoindazole

Produkt 1

HCID 30288931H-Indazole-1-propanamine, 3-amino-N,N-diethyl-Ausbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 70 ml of ethyl alcohol was added 3.30 g of 1-(3-diethylaminopropyl)-3-phthalimidoindazole. The mixture was added with 2.50 g of 85% hydrazine hydrate under cooling with ice and stirred for 3 hours under cooling with ice. The reaction mixture was filtered and the filtrate was condensed under reduced pressure. The condensed residue was added with 20 ml of water and the reaction product was extracted with chloroform. The chloroform layer was extracted with 2N-hydrochloric acid and the pH of the hydrochloric acid layer was adjusted to 10 with potassium carbonate. The alkali layer was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate, and chloroform was removed under reduced pressure to give 1.78 g of 1-(3-diethylaminopropyl)-3-aminoindazole having the following analytical values in a yield of 85%.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. filtrationThe reaction mixture was filtered
  4. customcondensed under reduced pressure
  5. extractionthe reaction product was extracted with chloroform
  6. extractionThe chloroform layer was extracted with 2N-hydrochloric acid
  7. extractionThe alkali layer was extracted with chloroform
  8. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate, and chloroform
  9. customwas removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0c7459f2a5e34fa9bff058192bae6290
Quelldatensatz
uspto-grants-1988_06
Patentnummer
US04751302

Notizen zur Reaktion

Wird geladen…