反应详情

To a solution of ethanesulfonic acid (5-bromo-pyridin-3-ylmethyl)-amide (intermediate A-11, 0.21 g, 0.752 mmol) in DMF (6 mL) cooled at 0° C. with an ice bath was added 60% NaH in mineral oil (0.039 g, 0.98 mmol) and the mixture was stirred for 15 min. Then, MeI (0.136 g, 0.96 mmol) was added and the reaction was stirred at 0° C. for another 15 min before being quenched with aq. ammonia (2 mL). The mixture was further diluted with brine and then extracted with EtOAc (2×15 mL). Combined organics were dried over Na2SO4, filtered and evaporated to dryness to give the title compound (0.209 g, 85%) as a yellow oil which was used with no further purification. MS: 293.1 and 295.1 (M+H+).

1. stirringthe reaction was stirred at 0° C. for another 15 min
2. custombefore being quenched with aq. ammonia (2 mL)
3. additionThe mixture was further diluted with brine
4. extractionextracted with EtOAc (2×15 mL)
5. dry with materialCombined organics were dried over Na2SO4
6. filtrationfiltered
7. customevaporated to dryness