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

HRID 1605

反应方程式

HRID 1605 反应方程式
[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

参与物

7

反应物 3

HCID 176醋酸HCID 517165乙酸铵HCID 19691073Diethyl 1-(6-chloro-1-oxoindan-2-yl)imidazole-2,4-dicarboxylate

产物 1

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

试剂、催化剂与溶剂 3

HCID 180丙酮溶剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 6342乙腈溶剂

实验过程

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).

后处理

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

来源与证据

ORD记录
ord-e4f280544c164e7781c5e91559bf59d4
来源数据集
uspto-grants-1998_03
专利号
US05726175

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