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90914-35-5

5-AMINO-3-(METHYLTHIO)-1H-PYRAZOLE-4-CARBOXAMIDE synthesis

2synthesis methods
-

Yield:90914-35-5 90%

Reaction Conditions:

Stage #1: 5-amino-3-(methylsulfanyl)-1H-pyrazole-4-carbonitrilewith sulfuric acid at 20;Cooling with ice;
Stage #2: with ammonia;water pH=8 - 9;Cooling with ice;

Steps:

2

5-Amino-3-(methylsulfanyl)-1H-pyrazole-4-carbonitrile (7.6 g) was added to concentrated sulfuric acid (25 ml) under ice-cooling, and the mixture was stirred at room temperature for five hours. The reaction solution was added dropwise to ice water (50 ml), and subsequently aqueous ammonia was added to precipitate crystals (pH 8 to 9). The precipitated solid was separated by filtration and dried to obtain 5-amino-3-(methylsulfanyl)-1H-pyrazole-4-carboxamide (colorless solid) (7.6 g, 90%). MS(ESI):173(M+H)+,171(M-H)- 1H NMR(600MHz,DMSO-D6)δppm 2.38(s,3H),6.00(bs,2H), 6.71(br,2H),11.84(br,1H)

References:

EP2123654,2009,A1 Location in patent:Page/Page column 18

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