HRID1443876

反应详情

EQUATION

反应方程式

REACTANTS

反应物

反应SMILES：COc1cnc(-c2cnc(C(=O)NC(C)(C)C)cn2)c2[nH]cc(C(=O)C(=O)N3CCN(C(=O)c4ccccc4)CC3)c12

HCID5280153

未命名化合物

PRODUCTS

产物

反应SMILES：COc1cnc(-c2cnc(C(N)=O)cn2)c2[nH]cc(C(=O)C(=O)N3CCN(C(=O)c4ccccc4)CC3)c12

HCID5280170

未命名化合物

收率 5.5%

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID1118

Sulfuric acid

H2O4S

溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

The compound of Example 15, 1-benzoyl-4-[(4-methoxy-7-(2-(1,1-dimethylethylaminocarbonyl)-pyrazin-5-yl)-6-azaindol-3-yl)-oxoacetyl]piperazine (20 mg) was dissolved in 1 drop of concentrated sulfuric acid. After 30 minutes, the mixture was diluted with 2 mL of methanol. The resulting solution was injected into a Shimadzu automated preparative HPLC System and the HPLC purification afforded the compound of Example 55, 1-benzoyl-4-[(4-methoxy-7-(2-aminocarbonyl-pyrazin-5-yl)-6-azaindol-3-yl)-oxoacetyl]piperazine (1 mg); MS m/z: (M+H)+ Calc'd for C26H24N7O5: 514.78; found 514.22. HPLC retention time: 1.44 minutes (column B).

WORKUP

后处理

customthe HPLC purification

来源与证据

来源类型: Open Reaction Database
ORD记录: ord-ced310fe17c24e0b970b7e19af4e2bc3
来源数据集: uspto-grants-2010_02
DOI: 10.6084/m9.figshare.5104873.v1
专利号: US07662823B2
来源说明: uspto-grants-2010_02

反应SMILES

[C:1]([N:9]1[CH2:14][CH2:13][N:12]([C:15](=[O:42])[C:16]([C:18]2[C:26]3[C:21](=[C:22]([C:29]4[N:30]=[CH:31][C:32]([C:35]([NH:37]C(C)(C)C)=[O:36])=[N:33][CH:34]=4)[N:23]=[CH:24][C:25]=3[O:27][CH3:28])[NH:20][CH:19]=2)=[O:17])[CH2:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>S(=O)(=O)(O)O.CO>[C:1]([N:9]1[CH2:14][CH2:13][N:12]([C:15](=[O:42])[C:16]([C:18]2[C:26]3[C:21](=[C:22]([C:29]4[N:30]=[CH:31][C:32]([C:35]([NH2:37])=[O:36])=[N:33][CH:34]=4)[N:23]=[CH:24][C:25]=3[O:27][CH3:28])[NH:20][CH:19]=2)=[O:17])[CH2:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1