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Hydrochloric Acid → 4-[(3R)-3,4-Dihydroxybutyl]-6-methoxypyrido[2,3-b]pyrazin-3(4H)-one

HRID 1847070
ノート
印刷プレビュー

反応式

HRID 1847070 の反応式
CC1(C)[O:6][C@H:5]([CH2:7][CH2:8][N:9]2[C:14](=[O:15])[CH:13]=[N:12][C:11]3[CH:16]=[CH:17][C:18]([O:20][CH3:21])=[N:19][C:10]2=3)[CH2:4][O:3]1.Cl>O1CCCC1>[OH:6][C@@H:5]([CH2:4][OH:3])[CH2:7][CH2:8][N:9]1[C:14](=[O:15])[CH:13]=[N:12][C:11]2[CH:16]=[CH:17][C:18]([O:20][CH3:21])=[N:19][C:10]1=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 867249934-{2-[(4R)-2,2-Dimethyl-1,3-dioxolan-4-yl]ethyl}-6-methoxypyrido[2,3-b]pyrazin-3(4H)-one

生成物 1

HCID 867249944-[(3R)-3,4-Dihydroxybutyl]-6-methoxypyrido[2,3-b]pyrazin-3(4H)-one収率 88.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

In tetrahydrofuran (100 ml) was dissolved 4-{2-[(4R)-2,2-dimethyl-1,3-dioxolan-4yl]ethyl}-6-methoxypyrido[2,3-b]pyrazin-3(4H)-one (2.55 g, 8.34 mmol), and 1N Hydrochloric acid aqueous solution (25 ml) was added thereto at room temperature and the mixture was stirred at 60° C. for 16 hours. After cooling in the air, the reaction solution was concentrated under reduced pressure and alkalized by adding 1N sodium hydroxide aqueous solution (30 ml) under cooling on ice. The solution was extracted with a lower layer solvent of chloroform/methanol/water (7:3:1) and the extract was dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure so as to yield 1.95 g (88%) of the title compound in the form of an orange solid.

後処理

  1. additionwas added
  2. temperatureAfter cooling in the air
  3. concentrationthe reaction solution was concentrated under reduced pressure
  4. additionby adding 1N sodium hydroxide aqueous solution (30 ml)
  5. temperatureunder cooling on ice
  6. extractionThe solution was extracted with a lower layer solvent of chloroform/methanol/water (7:3:1)
  7. dry with materialthe extract was dried over anhydrous sodium sulfate
  8. customThe solvent was removed under reduced pressure so as

出典と根拠

ORDレコード
ord-218131c99cd141158ab6e49814a3005f
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート