Maleic Acid → HCID 178481013, 화합물

HRID 897469

반응식

HRID 897469 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C@H:8]2[CH2:13][CH2:12][C@H:11]([N:14]3[C:18]4=[N:19][CH:20]=[N:21][C:22]([NH2:23])=[C:17]4[C:16]([C:24]4[CH:25]=[N:26][C:27]([O:30][C:31]5[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=5)=[N:28][CH:29]=4)=[N:15]3)[CH2:10][CH2:9]2)[CH2:4][CH2:3]1.[C:37]([OH:44])(=[O:43])/[CH:38]=[CH:39]\[C:40]([OH:42])=[O:41]>C(O)C>[C:37]([OH:44])(=[O:43])/[CH:38]=[CH:39]\[C:40]([OH:42])=[O:41].[C:37]([OH:44])(=[O:43])/[CH:38]=[CH:39]\[C:40]([OH:42])=[O:41].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C@H:8]2[CH2:13][CH2:12][C@H:11]([N:14]3[C:18]4=[N:19][CH:20]=[N:21][C:22]([NH2:23])=[C:17]4[C:16]([C:24]4[CH:25]=[N:26][C:27]([O:30][C:31]5[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=5)=[N:28][CH:29]=4)=[N:15]3)[CH2:10][CH2:9]2)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 444266Maleic AcidHCID 178481012HCID 178481012, 화합물

생성물 1

HCID 178481013HCID 178481013, 화합물수율 171.9%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of trans-1-[4-(4-methylpiperazino)cyclohexyl]-3-(2-phenoxy-5-pyrimidinyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (Int AX) (0.155 g, 0.00032 mol) in absolute ethanol (15 mL) was heated to reflux. A solution of maleic acid (0.148 g, 0.000128 mol) in absolute ethanol (10 mL) heated to 78° C. was added and the mixture was heated at reflux for 10 minutes. The mixture was allowed to cool to room temperature, and the white precipitate which formed was collected by filtration and washed with absolute ethanol (2×10 mL). The residual solvent was removed in vacuo to give trans-1-[4-(4-methylpiperazino)cyclohexyl]-3-(2-phenoxy-5-pyrimidinyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine bis maleate as a white solid (0.082 g, 0.00011 mol):

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 10 minutes
  4. customthe white precipitate which formed
  5. filtrationwas collected by filtration
  6. washwashed with absolute ethanol (2×10 mL)
  7. customThe residual solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-3626e9bc073f4cd4848c784b9c588079
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06921763B2

연결된 노트

불러오는 중…