Hydrochloric Acid → 3-(3-Methoxy-6-oxopyrido[2,3-b]pyrazin-5(6H)-yl)propanal

HRID 1847016

反応式

HRID 1847016 の反応式
[O:1]1CCO[CH:2]1[CH2:6][CH2:7][N:8]1[C:13]2=[N:14][C:15]([O:18][CH3:19])=[CH:16][N:17]=[C:12]2[CH:11]=[CH:10][C:9]1=[O:20].Cl>O1CCCC1>[CH3:19][O:18][C:15]1[N:14]=[C:13]2[N:8]([CH2:7][CH2:6][CH:2]=[O:1])[C:9](=[O:20])[CH:10]=[CH:11][C:12]2=[N:17][CH:16]=1

参加物

4

反応条件

温度
50 °C

実験手順

5-[2-(1,3-Dioxolan-2-yl)ethyl]-3-methoxypyrido[2,3-b]pyrazin-6(5H)-one (397 mg, 1.43 mmol) was dissolved in tetrahydrofuran (15 ml). To the solution was added a 1N hydrochloric acid aqueous solution (5 ml) under cooling on ice and the mixture was stirred at room temperature for two and a half hours and at 50° C. for 4 hours. After cooling in the air, the solvent was removed under reduced pressure and the residue was alkalized by adding saturated sodium bicarbonate water under cooling on ice. The resultant was extracted with dichloromethane, the extract was dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to yield 292 mg (87%) of the title compound in the form of a yellowish solid.

後処理

  1. temperatureunder cooling on ice
  2. temperatureAfter cooling in the air
  3. customthe solvent was removed under reduced pressure
  4. additionby adding saturated sodium bicarbonate water
  5. temperatureunder cooling on ice
  6. extractionThe resultant was extracted with dichloromethane
  7. dry with materialthe extract was dried over anhydrous sodium sulfate
  8. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-34d59c866ecf441c82864c3c65890d83
出典データセット
uspto-grants-2015_02
特許番号
US08952010B2

関連ノート

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