Sulfuric Acid → 1H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

HRID 459605

反応式

HRID 459605 の反応式
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[CH:4][C:3]=1[N:8]=O.[S:10](=[O:14])(=[O:13])([OH:12])[OH:11]>[Pd]>[S:10]([OH:14])([OH:13])(=[O:12])=[O:11].[NH2:8][C:3]1[CH:4]=[N:5][N:6]([CH3:7])[C:2]=1[NH2:1]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 128515805-Amino-1-methyl-4-nitrosopyrazole

生成物 1

HCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)収率 81%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

To a suspension of 5-amino-1-methyl-4-nitrosopyrazole (117 g) were added sulfuric acid (91 g) and 10% palladium on carbon (58 g). The mixture was hydrogenated under balloon pressure for 10 hours. The reaction mixture was filtered and the filtrate was concentrated in vacuo. To the concentrate was added isopropyl alcohol (2.3 L) and the mixture was stirred for 1 hour. The precipitated solid was collected by filtration and dried to give 4,5-diamino-1-methylpyrazole sulfate (158 g).

後処理

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. additionTo the concentrate was added isopropyl alcohol (2.3 L)
  4. filtrationThe precipitated solid was collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-1459ee86360e4a5983e2cbbf48c65e94
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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