Maleic Acid → GSK-2245035 maleate

HRID 2367968ノート

反応式

HRID 2367968 の反応式
[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

参加物

4

反応物 2

HCID 444266Maleic AcidHCID 44623937Gsk-2245035

生成物 1

HCID 53342522GSK-2245035 maleate収率 61.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-272fe083014a41e19c4783dd6e94a8a3
出典データセット
uspto-grants-2014_04
特許番号
US08703754B2

反応ノート

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