Ammonium Acetate → ethyl 4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate

HRID 1603

반응식

HRID 1603 반응식
C([O-])(=O)C.[NH4+:5].O=[C:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9][CH:8]1[N:16]1[CH:20]=[C:19]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:18]=[C:17]1[C:26]([O:28]CC)=O>C(O)(=O)C>[O:28]=[C:26]1[NH:5][C:7]2[C:15]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[CH2:9][C:8]=2[N:16]2[CH:20]=[C:19]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:18]=[C:17]12

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 19691065Diethyl 1-(1-oxoindan-2-yl)imidazole-2,4-dicarboxylate

생성물 1

HCID 19691063ethyl 4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate수율 37.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

51.2 g of ammonium acetate are added in small portions to a solution of 2 g of diethyl 1-(1-oxoindan-2-yl)imidazole-2,4-dicarboxylate in 80 ml of acetic acid and the mixture is heated to reflux for 2 hours. After cooling to a temperature close to 20° C. the precipitate formed is filtered off and rinsed with distilled water and then with methyl ethyl ketone (2×10 ml) to give 0.65 g of ethyl 4,5-dihydro-4-oxo-10H-imidazol[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate in the form of a beige solid melting above 260° C. (analysis % calculated C: 65.08, H: 4.44, N: 14.23; % found C: 65.2, H: 4.3, N: 13.8).

후처리

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 2 hours
  3. temperatureAfter cooling to a temperature
  4. customclose to 20° C. the precipitate
  5. customformed
  6. filtrationis filtered off
  7. washrinsed with distilled water

출처 및 근거

ORD 기록
ord-d0f3e38e8aab4374bc8286880e180242
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726175

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