Maleic Acid → 1-[1-(4-piperidyl)-4-piperidyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine, trimaleate salt

HRID 432139노트

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HRID 432139 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[CH2:12][CH2:11][CH:10]([N:13]3[C:17]4=[N:18][CH:19]=[N:20][C:21]([NH2:22])=[C:16]4[C:15]([C:23]4[CH:28]=[CH:27][C:26]([O:29][C:30]5[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=5)=[CH:25][CH:24]=4)=[N:14]3)[CH2:9][CH2:8]2)[CH2:3][CH2:2]1.[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40]>C(O)C>[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[C:36]([OH:43])(=[O:42])/[CH:37]=[CH:38]\[C:39]([OH:41])=[O:40].[NH:1]1[CH2:2][CH2:3][CH:4]([N:7]2[CH2:12][CH2:11][CH:10]([N:13]3[C:17]4=[N:18][CH:19]=[N:20][C:21]([NH2:22])=[C:16]4[C:15]([C:23]4[CH:28]=[CH:27][C:26]([O:29][C:30]5[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=5)=[CH:25][CH:24]=4)=[N:14]3)[CH2:9][CH2:8]2)[CH2:5][CH2:6]1

참가 물질

4

반응물 2

HCID 444266Maleic AcidHCID 223469961-[1-(4-piperidinyl)-4-piperidinyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine

생성물 1

HCID 1317242371-[1-(4-piperidyl)-4-piperidyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine, trimaleate salt수율 82.4%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

1-[1-(4-piperidyl)-4-piperidyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (108 mg, 0.230 mmol) was dissolved in 25 ml of ethanol and maleic acid (80 mg, 0.690 mmol) in 5 ml of hot ethanol was added. After 2 hours at room temperature, the solid was filtered and dried to give 155 mg of 1-[1-(4-piperidyl)-4-piperidyl]-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine, trimaleate salt. 1H NMR (DMSO) 1.80 (m, 2H), 2.42 (m, 4), 2.51 (m, 2H), 2.95 (m, 3H), 3.44 (bm, 7H), 5.06 (m, 1H), 6.10 (s, 6H), 7.15 (m, 5H), 7.45 (m, 2H), 7.67 (d, J=8.5 Hz, 2H), 8.27 (s, 1H); LC/MS (MH+32 484).

후처리

  1. filtrationthe solid was filtered
  2. customdried

출처 및 근거

ORD 기록
ord-3d8c58baad8b486ab4c757516110fc17
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660744B1

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