Sodium Hydroxide → 5-Amino-1-methyl-4-phenoxycarbonylaminopyrazole

HRID 459606

Reaktionsgleichung

Reaktionsgleichung von HRID 459606
S(O)(O)(=O)=O.[NH2:6][C:7]1[CH:8]=[N:9][N:10]([CH3:13])[C:11]=1[NH2:12].[OH-].[Na+].O1CCOCC1.Cl[C:23]([O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:24]>O>[NH2:12][C:11]1[N:10]([CH3:13])[N:9]=[CH:8][C:7]=1[NH:6][C:23]([O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:24]

Komponenten

6

Edukt 4

HCID 14798Sodium Hydroxide2×HCID 15891Phenyl chloroformateHCID 312751,4-DioxaneHCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

Produkt 1

HCID 219044605-Amino-1-methyl-4-phenoxycarbonylaminopyrazoleAusbeute 88,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 4,5-diamino-1-methylpyrazole sulfate (158 g) in water (1.1 L) was neutralized to pH 6.9 with 4N aqueous sodium hydroxide solution, and dioxane (474 ml) was added to this solution. To the resulting mixture was added dropwise phenyl chloroformate (124 g) maintaining pH of the mixture at 6.9 with 4N aqueous sodium hydroxide solution at a temperature below 10° C. The reaction mixture was stirred for 1 hour. The precipitated solid was collected by filtration and dried to give 5-amino-1-methyl-4-phenoxycarbonylaminopyrazole (155 g).

Aufarbeitung

  1. additionwas added to this solution
  2. filtrationThe precipitated solid was collected by filtration
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b8cf7690c27a47429de8e16d9808c19f
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07192943B2

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