Maleic Acid → GSK-2245035 maleate

HRID 2367968노트

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HRID 2367968 반응식
[NH2:1][C:2]1[N:10]=[C:9]([O:11][C@@H:12]([CH3:16])[CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:28])[N:6]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33]>C(O)(C)C>[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]\[C:32]([OH:34])=[O:33].[NH2:1][C:2]1[N:10]=[C:9]([O:11][C@@H:12]([CH3:16])[CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[NH:4][C:5](=[O:28])[N:6]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1

참가 물질

4

반응물 2

HCID 444266Maleic AcidHCID 44623937Gsk-2245035

생성물 1

HCID 53342522GSK-2245035 maleate수율 61.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
40 °C

실험 절차

6-amino-2-{[(1S)-1-methylbutyl]oxy}-9-[5-(1-piperidinyl)pentyl]-7,9-dihydro-8H-purin-8-one (for example, as prepared for Reference Example 1) (0.384 g, 0.98 mmol) was dissolved in isopropyl alcohol (4.6 mL, 12 vols) and heated to 40° C. Maleic acid (0.114 g, 0.98 mmol) was added. A clear solution was obtained. During cooling to room temperature, precipitation occurred. The slurry was filtered, washing with isopropyl alcohol (5 mL) and dried under reduced pressure at 40° C. to constant weight. 6-amino-2-{[(1S)-1-methylbutyl]oxy}-9-[5-(1-piperidinyl)pentyl]-7,9-dihydro-8H-purin-8-one, maleate salt (0.305 g, 61% th) was obtained as a white solid.

후처리

  1. customA clear solution was obtained
  2. temperatureDuring cooling to room temperature
  3. customprecipitation
  4. filtrationThe slurry was filtered
  5. washwashing with isopropyl alcohol (5 mL)
  6. customdried under reduced pressure at 40° C. to constant weight

출처 및 근거

ORD 기록
ord-272fe083014a41e19c4783dd6e94a8a3
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703754B2

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