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Formic Acid → HCID 13175327, 화합물

HRID 2418217
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HRID 2418217 반응식
[CH:1](O)=[O:2].C(N1C=CN=C1)(N1C=CN=C1)=O.[O:16]=[C:17]1[N:22]2[C:23]3[C:28]([NH:29][CH2:30][C:21]2=[N:20][CH:19]=[C:18]1[C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:27][CH:26]=[CH:25][CH:24]=3.C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH:1]([N:29]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[N:22]2[C:17](=[O:16])[C:18]([C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:19][N:20]=[C:21]2[CH2:30]1)=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 682631,1'-CarbonyldiimidazoleHCID 516892Sodium BicarbonateHCID 13175315HCID 13175315, 화합물

생성물 1

HCID 13175327HCID 13175327, 화합물수율 67%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 700 mg of formic acid (98%) in 70 ml of CH2Cl2 was stirred at room temperature under nitrogen while 100 mg of carbonyldiimidazole were added thereto. After 30, minutes 1.5 g of ethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate were added thereto and the mixture was stirred for another 6 hours. Then, the solution was poured into an aqueous NaHCO3 solution and extracted with ethyl acetate. The organic layer was dried over MgSO4, decolorized with charcoal and evaporated to dryness. The residue was crystallized from ethyl acetate to obtain 1.1 g (67% yield) of ethyl 5,6-dihydro-6-formyl-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate melting at 172°-4° C.

후처리

  1. additionwere added
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over MgSO4
  4. customevaporated to dryness
  5. customThe residue was crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-32914cbb66e049fcb1ff7cb2221fb5c5
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04472401

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