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Hydrochloric Acid → HCID 13175315, 화합물

HRID 2418215
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HRID 2418215 반응식
[O:1]=[C:2]1[N:7]2[C:8]3[C:13]([N:14]=[CH:15][C:6]2=[N:5][CH:4]=[C:3]1[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=3.Cl.C([O-])(O)=O.[Na+]>C(OCC)(=O)C.[Pd]>[O:1]=[C:2]1[N:7]2[C:8]3[C:13]([NH:14][CH2:15][C:6]2=[N:5][CH:4]=[C:3]1[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 12354442Ethyl 1-oxo-1H-pyrimido[1,2-A]quinoxaline-2-carboxylate

생성물 1

HCID 13175315HCID 13175315, 화합물수율 83.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate
용매

실험 절차

5.0 g of ethyl 1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate [Hermecz et al., J. Chem. Soc. Perkin I, 789 (1977)] were dissolved in 400 ml of ethyl acetate and 1.0 ml of HCl was added thereto followed by 300 mg of 5% Pd-C. The mixture obtained was hydrogenated for 5 hours at room temperature and atmospheric pressure. On completion of the reaction, the solution was made alkaline with NaHCO3 solution addition and filtered over celite. The organic phase was dried over MgSO4 and evaporated to dryness under nitrogen at 35° C. to obtain 4.2 g (83% yield) of ethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate melting at≃170° C.

후처리

  1. customThe mixture obtained
  2. customOn completion of the reaction
  3. filtrationfiltered over celite
  4. dry with materialThe organic phase was dried over MgSO4
  5. customevaporated to dryness under nitrogen at 35° C.

출처 및 근거

ORD 기록
ord-6938683f1805406e8056cec972a00db9
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04472401

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