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ChemicalBook CAS DataBase List 5-aMino-1-(4,4-difluorocyclohexyl)-1H-pyrazole-4-carboxaMide
1082745-54-7

5-aMino-1-(4,4-difluorocyclohexyl)-1H-pyrazole-4-carboxaMide synthesis

4synthesis methods
5-aMino-1-(4,4-difluorocyclohexyl)-1H-pyrazole-4-carbonitrile

1082745-53-6
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5-aMino-1-(4,4-difluorocyclohexyl)-1H-pyrazole-4-carboxaMide

1082745-54-7
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Yield:1082745-54-7 68%

Reaction Conditions:

with ammonia;dihydrogen peroxide in ethanol;water at 20; for 2.16667 h;

Steps:

4A

Example 4A; 3.88 g (14.6 mmol) of Example 3A were mixed with 40 ml_ of ethanol. At room temperature a solution of 35 ml_ (0.41 mol) hydrogen peroxide (35 % in water) in 20 ml_ ammonia (25 % in water) was added over a period of 10 min. The reaction mixture was stirred at room temperature for 2h. The solution was concentrated to a volume of 50 ml_ under reduced pressure. The residue was mixed withdichloromethane and water. The organic layer was extracted with water and 40 % Na2S2θ3 solution. The organic layer was dried, filtered and the filtrate was concentrated under reduced pressure. 2.44 g (68 %) of the product were obtained. HPLC-MS (Method 1 ): R1 = 0.91 minMS (ESI pos): m/z = 245 (M+H)+

References:

WO2011/18495,2011,A1 Location in patent:Page/Page column 76