Acetic Acid → ethyl 7-chloro-4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate

HRID 1605

반응식

HRID 1605 반응식
[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH:7]([N:12]3[CH:16]=[C:15]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[N:14]=[C:13]3[C:22]([O:24]CC)=O)[C:8]2=O)=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+:31].C(O)(=O)C>C(#N)C.CO.CC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:6][C:7]3[N:12]4[CH:16]=[C:15]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[N:14]=[C:13]4[C:22](=[O:24])[NH:31][C:8]=3[C:9]=2[CH:10]=1

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 517165Ammonium AcetateHCID 19691073Diethyl 1-(6-chloro-1-oxoindan-2-yl)imidazole-2,4-dicarboxylate

생성물 1

HCID 19691067ethyl 7-chloro-4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate수율 61.7%

시약·촉매·용매 3

HCID 180Acetone용매HCID 887Methanol용매HCID 6342Acetonitrile용매

실험 절차

The procedure is as in Example 1 but starting from 5 g of diethyl 1-(6-chloro-1-oxoindan-2-yl)imidazole-2,4-dicarboxylate, 118 g of ammonium acetate and 190 ml of acetic acid. After washing the precipitate with water and then with methyl ethyl ketone, the solid obtained is first of all ground in acetonitrile and then in methanol and finally in acetone to obtain 2.7 g of ethyl 7-chloro-4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate in the form of a brown solid melting above 260° C. (analysis % calculated C: 58.28, H: 3.67, Cl: 10.75, N: 12.74; % found C: 58.6, H: 3.4, Cl: 10.4, N: 13.1).

후처리

  1. washAfter washing the precipitate with water
  2. customwith methyl ethyl ketone, the solid obtained

출처 및 근거

ORD 기록
ord-e4f280544c164e7781c5e91559bf59d4
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726175

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