反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of sodium hydride (70.6 mg, 2.94 mmol) and 1H-1,2,4-triazole (203 mg, 2.94 mmol) in NMP (1 mL) was added cis-4-(5-chloro-2-nitrophenylamino)-N-isopropylcyclohexanecarboxamide (100 mg, 0.294 mmol). The resulting suspension was irradiated in a microwave reactor for 1 hour at 150° C. The reaction mixture was partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc (×2). The combined organic layers were then washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated to provide a yellow oil that crystallized upon standing to provide cis-N-isopropyl-4-(2-nitro-5-(1H-1,2,4-triazol-1-yl)phenylamino)cyclohexanecarboxamide as a yellow solid (100 mg, 91% yield).
WORKUP
后处理
- customThe resulting suspension was irradiated in a microwave reactor for 1 hour at 150° C
- customThe reaction mixture was partitioned between water and EtOAc
- extractionThe aqueous layer was extracted with EtOAc (×2)
- washThe combined organic layers were then washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto provide a yellow oil that
- customcrystallized