HRID517767
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
To a solution of 5-(chloromethyl)-1-[3-(trifluoromethyl)phenyl]-1H-tetrazole (200 mg, 0.762 mmol, commercially available from Otava, Kiev, Ukraine) in acetonitrile (3 mL) was added triethylamine (0.318 mL, 2.285 mmol) and 3-methyl-2-piperazinone (87 mg, 0.762 mmol, Sigma-Aldrich). The reaction mixture was heated to 120° C. for 20 min in a microwave reactor. The reaction mixture was concentrated in vacuo. The crude product was purified by silica chromatography (Biotage SP4), eluting with an increasing gradient of (2N NH3 in MeOH) in DCM. The relevant fractions were combined and concentrate to give the title compound as white crystals (151 mg)
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- customThe crude product was purified by silica chromatography (Biotage SP4)
- washeluting with an increasing gradient of (2N NH3 in MeOH) in DCM
- concentrationconcentrate