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

HRID 432139ノート

反応式

HRID 432139 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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).

後処理

  1. filtrationthe solid was filtered
  2. customdried

出典と根拠

ORDレコード
ord-3d8c58baad8b486ab4c757516110fc17
出典データセット
uspto-grants-2003_12
特許番号
US06660744B1

反応ノート

読み込み中…