HRID1375417

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID176

Acetic Acid

C2H4O2

结构：CCN(CC)C(=O)c1ccc(Nc2ncc(N)c(NC)n2)cc1

HCID58786782

未命名化合物

HCID58786806

未命名化合物

PRODUCTS

生成物

结构：CCN(CC)C(=O)c1ccc(Nc2ncc3nc(-c4c(Cl)c(OC)nc(OC)c4Cl)c(=O)n(C)c3n2)cc1

HCID9872467

未命名化合物

收率 56%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8019

2-Methoxyethanol

C3H8O2

溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

A mixture of 0.47 g (1.5 mmol) of 5-amino-2-[[4-(diethylaminocarbonyl)-phenyl]amino]-4-(methylamino)pyrimidine, 0.62 g (2 mmol) of ethyl 2-(3,5-dichloro-2,6-dimethoxypyridin-4-yl)-2-oxoacetate and 1.0 mL of HOAc in 20 mL of 2-methoxyethanol is heated under reflux for 16 hours. Workup in EtOAc, followed by chromatography on silica, eluting with hexane/EtOAc (1:1), gives 0.42 g (56%) of the title compound (Compound 22): mp (EtOH) 274–276° C.

WORKUP

后处理

temperatureis heated
temperatureunder reflux for 16 hours
washeluting with hexane/EtOAc (1:1)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-726f9ae4cf564924923ad09410c4131c
来源数据集: uspto-grants-2007_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07169778B2
来源说明: uspto-grants-2007_01

反应 SMILES

[NH2:1][C:2]1[C:3]([NH:22][CH3:23])=[N:4][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]([N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])=[O:16])=[CH:11][CH:10]=2)=[N:6][CH:7]=1.[Cl:24][C:25]1[C:26]([O:41][CH3:42])=[N:27][C:28]([O:39][CH3:40])=[C:29]([Cl:38])[C:30]=1[C:31](=O)[C:32]([O:34]CC)=O.CC(O)=O>COCCO.CCOC(C)=O>[Cl:38][C:29]1[C:28]([O:39][CH3:40])=[N:27][C:26]([O:41][CH3:42])=[C:25]([Cl:24])[C:30]=1[C:31]1[C:32](=[O:34])[N:22]([CH3:23])[C:3]2[N:4]=[C:5]([NH:8][C:9]3[CH:10]=[CH:11][C:12]([C:15]([N:17]([CH2:18][CH3:19])[CH2:20][CH3:21])=[O:16])=[CH:13][CH:14]=3)[N:6]=[CH:7][C:2]=2[N:1]=1