反应详情

To a solution of 2,2-dimethyl-3,4-dihydro-2H-chromene-8-carboxylic acid (300 mg, 1.45 mmol) in methanol (2.10 mL) and toluene (5.20 mL) cooled to 0° C. was added TMS-diazomethane (1.82 mL, 3.64 mmol) dropwise via a syringe. The reaction mixture was warmed to room temperature and stirred for 45 minutes. It was then cooled to 0° C., and acetic acid (2.00 mL) was added carefully. The solvent was evaporated under vacuum and the residue was re-dissolved in EtOAc (80.0 mL), washed with a saturated NaHCO3 solution (20.0 mL, dried over Na2SO4, filtered and concentrated under vacuum. The crude product was used directly to the next step without further purification.

1. temperatureIt was then cooled to 0° C.
2. customThe solvent was evaporated under vacuum
3. dissolutionthe residue was re-dissolved in EtOAc (80.0 mL)
4. washwashed with a saturated NaHCO3 solution (20.0 mL
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customThe crude product was used directly to the next step without further purification