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

HRID 459606

반응식

HRID 459606 반응식
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]

참가 물질

6

반응물 4

HCID 14798Sodium Hydroxide2회HCID 15891Phenyl chloroformateHCID 312751,4-DioxaneHCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

생성물 1

HCID 219044605-Amino-1-methyl-4-phenoxycarbonylaminopyrazole수율 88.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-b8cf7690c27a47429de8e16d9808c19f
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192943B2

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