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

HRID 1577806

반응식

HRID 1577806 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 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 in 200 ml. of anhydrous ethanol was prepared. A 17.4 g. batch of diethyl 2-ketomalonate were 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-a2b01a3b860942888662a28af9a29fcf
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04289773

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