反应详情

To a solution of amide from Example 417 (60 mg, 0.14 mmol) in THF (2 ml) at 0° C. was added ethynylmagnesium bromide (0.5 M in THF, 1.4 ml, 0.7 mmol). The reaction mixture was warmed to rt for 2 h, then heated at 50° C. for 2 h, and at rt overnight. Diluted with ether, washed with saturated NaHCO3, dried with Na2SO4. Concentrated in vacuo and purified by prep. TLC to give the title compound (30 mg, 32%) (5% MeOH—CHCl3). It has a retention time of 6.82 min (standard LCl method, 8 min run). LCMS Found: (M+H)+=393.2

1. temperatureheated at 50° C. for 2 h
2. customat rt
3. customovernight
4. washwashed with saturated NaHCO3
5. dry with materialdried with Na2SO4
6. concentrationConcentrated in vacuo
7. custompurified by prep