Dichloromethane → HCID 68756523, 화합물

반응식

COC1C=CC(C[N:8]2[C:12]3=[N:13][CH:14]=[C:15]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)[C:16]([N:17]4[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]4)=[C:11]3[CH:10]=[N:9]2)=CC=1.C(O)(C(F)(F)F)=O.C(Cl)[Cl:46]>>[ClH:46].[ClH:46].[C:30]1([C:15]2[C:16]([N:17]3[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]3)=[C:11]3[CH:10]=[N:9][NH:8][C:12]3=[N:13][CH:14]=2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

참가 물질

반응물 3

HCID 6344Dichloromethane

HCID 6422Trifluoroacetic acid2회

HCID 68764155tert-butyl 4-(1-(4-methoxybenzyl)-5-phenyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate

생성물 1

HCID 68756523HCID 68756523, 화합물수율 75%

실험 절차

A solution of tert-butyl 4-(1-(4-methoxybenzyl)-5-phenyl-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (0.440 g, 0.881 mmol) in DCM (5 mL) was added to TFA (1 mL) and stirred at room temperature for 1 hour. The reaction was then concentrated to dryness and dried under vacuum for 1 hour. TFA (3.39 mL, 44.0 mmol) was then added, and the mixture was stirred at 65° C. for 4 hours. The reaction was then concentrated to dryness, and the resulting residue was dissolved in DCM (3 mL). HCl in ether (2 mL, 2N) and ether (10 mL) were then added, and the resulting solid was collected by filtration to give 5-phenyl-4-(piperazin-1-yl)-1H-pyrazolo[3,4-b]pyridine dihydrochloride (0.29 g, 75%). MS ESI (+) m/z 280.1 detected.