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Acetic Acid → 4-Oxo-4H-pyrimido[2,1-a]isoquinoline-3-carboxylic Acid

HRID 1704813
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반응식

HRID 1704813 반응식
N=[C:2]1[N:7]2[CH:8]=[CH:9][C:10]3[C:15]([C:6]2=[N:5][CH:4]=[C:3]1[C:16]([O:18]CC)=[O:17])=[CH:14][CH:13]=[CH:12][CH:11]=3.C(O)(=[O:23])C>Cl.O>[O:23]=[C:2]1[N:7]2[CH:8]=[CH:9][C:10]3[C:15]([C:6]2=[N:5][CH:4]=[C:3]1[C:16]([OH:18])=[O:17])=[CH:14][CH:13]=[CH:12][CH:11]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 22758844ethyl 4-imino-4H-pyrimido[2,1-a]isoquinoline-3-carboxylate

생성물 1

HCID 227588274-Oxo-4H-pyrimido[2,1-a]isoquinoline-3-carboxylic Acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

A solution of ethyl 4-imino-4H-pyrimido[2,1-a]isoquinoline-3-carboxylate (1.0 g.) in acetic acid (20 ml.) and 37% hydrochloric acid (20 ml.) was refluxed for 35 minutes. The solution was cooled and diluted with H2O to precipitate the crude acid (760 mg.), m.p. 219°-231° (prior softening). Recrystallized material (2-methoxyethanol) and a m.p. of 249°-252° and mixed melting point of 252°-255° with product from Example 2.

후처리

  1. temperatureThe solution was cooled
  2. customto precipitate the crude acid (760 mg.), m.p. 219°-231° (prior softening)
  3. additionRecrystallized material (2-methoxyethanol) and a m.p. of 249°-252° and mixed melting point of 252°-255° with product from Example 2

출처 및 근거

ORD 기록
ord-c73e0f591eed410db64987fb6f9e5957
출처 데이터셋
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04127720

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