Hydrazine → 2-(2-aminoethyl)-6-phenylpyridazin-3(2H)-one

HRID 1878742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1878742
[O:1]=[C:2]1[N:7]([CH2:8][CH2:9][N:10]2C(=O)C3C(=CC=CC=3)C2=O)[N:6]=[C:5]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:4]=[CH:3]1.NN>CO>[NH2:10][CH2:9][CH2:8][N:7]1[C:2](=[O:1])[CH:3]=[CH:4][C:5]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[N:6]1

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 13103521HCID 13103521, Verbindung

Produkt 1

HCID 129026032-(2-aminoethyl)-6-phenylpyridazin-3(2H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

A mixture of 2-(2-(6-oxo-3-phenylpyridazin-1(6H)-yl)ethyl)isoindoline-1,3-dione (2.1 g, 6.1 mmol) and hydrazine (10 mL, 10.0 mmol) (THF) in MeOH (40 mL) was heated to 75° C. A clear solution was formed. After overnight (18 h), the slurry was cooled to room temperature and was filtered and washed with MeOH. The filtrate was concentrated and washed with 20% MeOH/CH2Cl2 to give a yellow solid (LCMS indicated the presence of product). The filtrate was concentrated under vacuum and was carried to next step.

Aufarbeitung

  1. customA clear solution was formed
  2. temperaturethe slurry was cooled to room temperature
  3. filtrationwas filtered
  4. washwashed with MeOH
  5. concentrationThe filtrate was concentrated
  6. washwashed with 20% MeOH/CH2Cl2
  7. customto give a yellow solid (LCMS
  8. concentrationThe filtrate was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-06085f8a8f524b67a71ae8284e771fcb
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08314087B2

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