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

HRID 459605노트

반응식

HRID 459605 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1459ee86360e4a5983e2cbbf48c65e94
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192943B2

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