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Dimethylformamide → HCID 13175316, 화합물

HRID 2418216
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HRID 2418216 반응식
CN(C)C=O.Cl[C:7]([O:9][CH2:10][CH3:11])=[O:8].[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([NH:25][CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3>O>[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([N:25]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 10928Ethyl chloroformateHCID 13175315HCID 13175315, 화합물

생성물 1

HCID 13175316HCID 13175316, 화합물수율 41%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4 ml of dry dimethylformamide were saturated with nitrogen for 10 minutes before 150 mg of ethyl chloroformate and 280 mg of ethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate were added thereto. The solution obtained was left at room temperature overnight and then was poured into water. The mixture was extracted with ethyl acetate and the organic phase was dried over MgSO4 and evaporated to dryness. The residue was chromatographed over silica gel and eluted with ethyl acetate to obtain 140 mg (41% yield) of diethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2,6-dicarboxylate melting at 140°-2° C.

후처리

  1. additionwere added
  2. customThe solution obtained
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organic phase was dried over MgSO4
  5. customevaporated to dryness
  6. customThe residue was chromatographed over silica gel
  7. washeluted with ethyl acetate

출처 및 근거

ORD 기록
ord-a24dfdf9a5314ed18eb735361453d567
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04472401

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