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1,3-Diethyl 2-oxopropanedioate → Ethyl 6,7-dichloro-3-hydroxyquinoxaline-2-carboxylate

HRID 1414078
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HRID 1414078 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH2:9])=[C:4]([NH2:10])[CH:3]=1.O=[C:12]([C:18](OCC)=[O:19])[C:13]([O:15][CH2:16][CH3:17])=[O:14]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[Cl:8])[N:9]=[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:18](=[O:19])[NH:10]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 691051,3-Diethyl 2-oxopropanedioateHCID 792974,5-Dichloro-1,2-phenylenediamine

생성물 1

HCID 6320212Ethyl 6,7-dichloro-3-hydroxyquinoxaline-2-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 17.7 g. of 4,5-dichloro-o-phenylenediamine and 200 ml. of anhydrous ethanol was prepared. A 17.4 g. batch of diethyl 2-keto-malonate was added to this solution and the mixture was heated to refluxing temperature for about 17 hours. The volatile constituents were removed by evaporation in vacuo. Recrystallization of the residue from ethanol yielded 20 g. of ethyl 6,7-dichloro-3,4-dihydro-3-oxo-2-quinoxaline carboxylate formed in the above reaction; melting in the range 226°-227° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto refluxing temperature for about 17 hours
  3. customThe volatile constituents were removed by evaporation in vacuo
  4. customRecrystallization of the residue from ethanol
  5. customyielded 20 g

출처 및 근거

ORD 기록
ord-9d7af4864aa945d8b64aadf1d2e5340a
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04252954

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