反应详情

温度

70 °C

To a solution of 70 mg rac-(3-Hydroxymethyl-pyrrolidin-1-yl)-[5-methanesulfonyl-2-((S)-2,2,2-trifluoro-1-methyl-ethoxy)-phenyl]-methanone (Example C1) in 1.4 ml tetrahydrofuran were added 30 mg 4-hydroxybenzotrifluoride and 50 mg diphenyl-2-pyridylphosphine. 43 mg Di-tert-butyl azodicarboxylate was added. The mixture was stirred at 70° C. for 23 hours. The solvent was removed in vacuo. The oil was purified on silica gel (eluent: ethyl acetate) to yield a yellow gum. The gum was dissolved in ethyl acetate. The solution was washed 3 times with HCl 5N, once with water, dried over Na2SO4, filtered and concentrated in vacuo to provide the title compound as a light yellow foam. MS (m/e): 540.3 (M+H+, 100%).

1. customThe solvent was removed in vacuo
2. customThe oil was purified on silica gel (eluent: ethyl acetate)
3. customto yield a yellow gum
4. washThe solution was washed 3 times with HCl 5N
5. dry with materialonce with water, dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo