反应详情

温度

-20 °C

To a solution of compound 126 (schemes 6 or 9) (200 mg, 0.381 mmol) in dry tetrahydrofuran (8 mL) under nitrogen at −20° C. was added 4-nitrophenyl chloroformate (115 mg, 0.572 mmol). The reaction mixture was stirred at −20° C. for 2 h. A solution of 3-(dimethylphosphoryl)aniline 287 (97 mg, 0.57 mmol) and N,N′-diisopropylethylamine (0.200 mL, 1.14 mmol) in a mixture of dry tetrahydrofuran (2 mL) and dry N,N′-dimethylformamide (2 mL) were added at −20° C., the reaction mixture was allowed to warm to room temperature slowly, and the stirring was continued for an additional 16 h. The solvent was removed under reduced pressure; the residue was diluted with ethyl acetate, washed with a saturated aqueous solution of ammonium chloride, dried over anhydrous sodium sulfate and concentrated. Purification via Biotage (linear gradient 0-20%, methanol/dichloromethane; 25M column) afforded compound 288 (230 mg, 0.32 mmol, 84%). MS (m/z): 720.4 (M+H).

1. additionwere added at −20° C.
2. temperatureto warm to room temperature slowly
3. waitthe stirring was continued for an additional 16 h
4. customThe solvent was removed under reduced pressure
5. additionthe residue was diluted with ethyl acetate
6. washwashed with a saturated aqueous solution of ammonium chloride
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated
9. customPurification via Biotage (linear gradient 0-20%, methanol/dichloromethane; 25M column)