反应详情

To a suspension of NaH (60%, 99 mg) in THF (dry) (10 mL) was added 2-chloroethanesulfonyl chloride (0.156 mL) at 0° C. and the mixture was stirred for 10 min at the same temperature. A solution of 3-(4-(3,4-dimethylphenoxy)phenyl)pyridin-2-amine (144 mg) in THF (dry) (10 mL) was added at 0° C. and the mixture was stirred at room temperature under nitrogen overnight. The mixture was quenched with water at 0° C. and extracted with EtOAc/THF. Silica-gel was added to the organic phase and the volatiles were removed in vacuo. The mixture supported on silica-gel was purified by column chromatography (silica gel, eluted with MeOH in EtOAc) to give the title compound (119.7 mg). A part of product was recrystallized from MeCN/IPE.

1. stirringthe mixture was stirred at room temperature under nitrogen overnight
2. customThe mixture was quenched with water at 0° C.
3. extractionextracted with EtOAc/THF
4. additionSilica-gel was added to the organic phase
5. customthe volatiles were removed in vacuo
6. customwas purified by column chromatography (silica gel, eluted with MeOH in EtOAc)