Hydrochloric Acid → 4-(4-bromophenyl)-3-methyl-4,5-dihydro-1H-1,2,4-triazol-5-one

HRID 1484507

Reaktionsgleichung

Reaktionsgleichung von HRID 1484507
[C:1]([NH:4][NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][CH:10]=1)=[O:7])(=O)[CH3:2].[OH-].[Na+].Cl>O>[Br:15][C:12]1[CH:13]=[CH:14][C:9]([N:8]2[C:1]([CH3:2])=[N:4][NH:5][C:6]2=[O:7])=[CH:10][CH:11]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 232741832-acetyl-N-(4-bromophenyl)hydrazinecarboxamide

Produkt 1

HCID 14877914-(4-bromophenyl)-3-methyl-4,5-dihydro-1H-1,2,4-triazol-5-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A large microwave tube was filled in with 2-acetyl-N-(4-bromophenyl)hydrazinecarboxamide (1.8 g, 6.62 mmol) and 2M aqueous NaOH (9 mL, 18 mmol). The reaction mixture was heated under microwave irradiation for 20 min at 130° C. Water (ca 18 mL) was added and the pH was adjusted to 4 by dropwise addition of aqueous HCl, with stirring. The thick precipitate was collected by filtration, washed with small amounts of cold water and dried. A small amount (220 mg) was purified by analytical preparation leading to 195 mg of the title compound.

Aufarbeitung

  1. filtrationThe thick precipitate was collected by filtration
  2. washwashed with small amounts of cold water
  3. customdried
  4. customA small amount (220 mg) was purified by analytical preparation

Quellen und Nachweise

ORD-Eintrag
ord-ed06d3196331403db184342ecda5e251
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09422252B2

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