反应详情

To an ice bath cooled mixture of EXAMPLE 1C (2.0 g) in THF (20 mL) was added 60% oily NaH (265 mg). The mixture was stirred for 30 minutes before adding chloromethyl methyl ether (0.54 mL). The mixture was stirred for 3 hours and overnight at room temperature, quenched by adding saturated NH4Cl mixture and extracted with diethylether. The extract was washed with water and brine and dried (Na2SO4), filtered and concentrated. The concentrate was purified with flash column chromotography on silica gel with 5% ethyl acetate/hexanes.

1. stirringThe mixture was stirred for 3 hours and overnight at room temperature
2. customquenched
3. additionby adding saturated NH4Cl mixture
4. extractionextracted with diethylether
5. washThe extract was washed with water and brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe concentrate was purified with flash column chromotography on silica gel with 5% ethyl acetate/hexanes