反应详情
EQUATION
反应方程式
REACTANTS
反应物
Hydrochloric Acid
ClH
4-Methylmorpholine
C5H11NO
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide
C8H17N3
1-Hydroxybenzotriazole
C6H5N3O
5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carboxylic acid
C17H11Cl3N2O2
未命名化合物
未命名化合物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a tert-butyl 2-cyclohexyl-2-oxoethylcarbamate (228 mg, 0.946 mmol) in DCM (5 mL) was added 4M HCl in 1,4-dioxane (5 mL) at room temperature. The reaction continued for an hour at room temperature. The volatiles were removed under vacuum. To the residue (2-amino-1-cyclohexylethanone hydrochloric acid), 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carboxylic acid (361 mg, 0.946 mmol), EDCI (272 mg, 1.429 mmol), HOBt (192 mg, 1.429 mmol) in DMF (9 mL) was added NMM (1.0 mL, 9.46 mmol) at room temperature. The reaction mixture was stirred at room temperature overnight. The residue was purified by reverse-phase prep HPLC to afford the title compound (232 mg, 49%).
WORKUP
后处理
- waitThe reaction continued for an hour at room temperature
- customThe volatiles were removed under vacuum
- customThe residue was purified by reverse-phase prep HPLC