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

HRID 459606

反応式

HRID 459606 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 219044605-Amino-1-methyl-4-phenoxycarbonylaminopyrazole収率 88.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b8cf7690c27a47429de8e16d9808c19f
出典データセット
uspto-grants-2007_03
特許番号
US07192943B2

関連ノート

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