HRID79098
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
Sodium hydride (26 mg, 0.66 mmol) was added to a stirred solution of 3-(4-tertbutylbenzamido)benzenesulfonic acid (0.10 g, 0.30 mmol) in THF (5 mL), and after 30 min iodomethane (37 μL, 0.60 mmol) was added. The reaction was stirred for 17 h, and 1 M aqueous hydrochloric acid (1 mL) was added. The solvent was removed under vacuum, and the residue was purified by preparative reverse phase HPLC using 10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA) to give 3-(4-tert-butyl-N-methylbenzamido)benzenesulfonic acid (24 mg, 23% yield). LC/MS: m/z 348.3 (M+H)+ at 3.82 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).
WORKUP
后处理
- customThe solvent was removed under vacuum
- customthe residue was purified by preparative reverse phase