反应详情

温度

0 °C

To a suspension of NaH (60% dispersion in mineral oil, 59 mg, 1.48 mmol) in DMF (2 mL) was slowly added a solution of 1H-indole-5-carboxylic acid methyl ester 19a (200 mg, 1.14 mmol) in DMF (1 mL) at 0° C. The resulting solution was stirred at 0° C. for 20 min and 1,1-difluoro-2-iodoethane 23a (263 mg, 1.37 mmol) was added. The reaction was warmed to room temperature and stirred for 2 h. The reaction was quenched with water and extracted with EtOAc. The organic layer was concentrated and purified by flash column chromatography (silica gel, 20% EtOAc/hexanes) to afford compound 23b.

1. temperatureThe reaction was warmed to room temperature
2. stirringstirred for 2 h
3. customThe reaction was quenched with water
4. extractionextracted with EtOAc
5. concentrationThe organic layer was concentrated
6. custompurified by flash column chromatography (silica gel, 20% EtOAc/hexanes)