HRID624783

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID66888

Benzenemethanamine, 3,4-dimethyl-

C9H13N

$结构：CS(=O)c1nc(NC2CC2)n2ncc(/C=C3\NC(=O)NC3=O)c2n1$

HCID178504622

未命名化合物

$结构：CS(=O)(=O)c1nc(NC2CC2)n2ncc(/C=C3\NC(=O)NC3=O)c2n1$

HCID178504850

未命名化合物

PRODUCTS

生成物

$结构：Cc1ccc(CNc2nc(NC3CC3)n3ncc(/C=C4\NC(=O)NC4=O)c3n2)cc1C$

HCID178425513

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID13387

N-Methyl-2-pyrrolidone

C5H9NO

3 次

CONDITIONS

反应条件

温度: 80 °C

PROCEDURE

实验过程

A solution of (3,4-dimethylphenyl)methanamine in NMP (106 μl, 0.4 M, 1.5 eq, 0.042 mmol) was transferred in a glass reaction vial. A solution of a (1:1) mixture of (Z)-5-((4-(cyclopropylamino)-2-(methylsulfonyl)pyrazolo[1,5-a][1,3,5]triazin-8-yl)methylene)imidazolidine-2,4-dione and (Z)-5-((4-(cyclopropylamino)-2-(methylsulfinyl)pyrazolo[1,5-a][1,3,5]triazin-8-yl)methylene)imidazolidine-2,4-dione in NMP (100 μl, 0.282M, 1.0 eq, 0.0282 mmol) was added. The mixture was heated at 80° C. for 5 hours. NMP was added (0.7 ml) and the solution subjected to preparative HPLC purification. Genevac evaporation provided (Z)-5-((4-(cyclopropylamino)-2-(3,4-dimethylbenzylamino)pyrazolo[1,5-a][1,3,5]triazin-8-yl)methylene)imidazolidine-2,4-dione as a solid (5.8 mg). LCMS (ES): >85% pure, m/z 419 [M+H]+.

WORKUP

后处理

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customthe solution subjected to preparative HPLC purification
customGenevac evaporation