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
4-Tert-butyl-2,6-dimethyl-benzenesulfonyl chloride (0.100 g, 0.383 mmol) was added to a solution of 2-methyl-3,5-bis(trifluoromethyl)aniline (0.094 g, 0.387 mmol) in dry pyridine (1 mL). The reaction was capped and stirred at room temperature for 1 day then stirred at 30° C. for 1 day. The reaction was then concentrated under vacuum. To this was added diethyl ether (60 mL) and the mixture was washed with 0.1 N HCl (3×20 mL) followed by 0.1 N NaOH (2×20 mL) then saturated NaCl (2×20 mL). After drying the organic layer over MgSO4, the solution was filtered and concentrated under vacuum. The crude compound was triturated with hexanes (3×10 mL) to afford the title compound (0.051 g, 28% yield). LCMS (M+Na) 490.
WORKUP
后处理
- customThe reaction was capped
- stirringthen stirred at 30° C. for 1 day
- concentrationThe reaction was then concentrated under vacuum
- additionTo this was added diethyl ether (60 mL)
- washthe mixture was washed with 0.1 N HCl (3×20 mL)
- dry with materialAfter drying the organic layer over MgSO4
- filtrationthe solution was filtered
- concentrationconcentrated under vacuum
- customThe crude compound was triturated with hexanes (3×10 mL)