Ethanol → 7,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine dihydrochloride

반응식

FC(F)(F)C(O)=O.[CH3:8][C:9]1([CH3:25])[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][C:11]2[CH:22]=[N:23][NH:24][C:10]1=2.C(O)C.[Cl:29]CCl>>[ClH:29].[ClH:29].[CH3:8][C:9]1([CH3:25])[CH2:14][NH:13][CH2:12][C:11]2[CH:22]=[N:23][NH:24][C:10]1=2

참가 물질

반응물 4

HCID 702Ethanol

HCID 6344Dichloromethane

HCID 6422Trifluoroacetic acid

HCID 37818370tert-Butyl 7,7-dimethyl-6,7-dihydro-1H-pyrazolo[4,3-c]pyridine-5(4H)-carboxylate

생성물 1

HCID 667221937,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine dihydrochloride

실험 절차

At 0° C. 5 mL trifluoroacetic acid was added to 1.60 g (6.05 mmol) tert-butyl 7,7-dimethyl-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-5-carboxylate (synthesised analogously to WO2005/065779) in 15 mL dichloromethane and the reaction mixture was stirred for 2 h at RT. Then the solvent was eliminated i. vac. The residue was combined with ethanol and evaporated down again i. vac. The residue was dissolved in ethanol and 12 mL of a 1.25 M ethanolic HCl solution were added. The mixture was again evaporated down i. vac. The residue was triturated with ethanol. The solid was suction filtered and dried.