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

HRID 1847016

반응식

HRID 1847016 반응식
[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

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 867249455-[2-(1,3-Dioxolan-2-yl)ethyl]-3-methoxypyrido[2,3-b]pyrazin-6 (5H)-one

생성물 1

HCID 867249463-(3-Methoxy-6-oxopyrido[2,3-b]pyrazin-5(6H)-yl)propanal수율 87.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-34d59c866ecf441c82864c3c65890d83
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952010B2

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