反应详情

To a stirred ice-cold solution of (27) (0.21 g., 1.0 mM) in dried methylene chloride (10 mL) containing anhydrous pyridine (0.3 mL) is added (7) (0.27 g., 1.03 mM), dissolved in 5 methylene chloride (5 mL), dropwise over 1 minute (some methylene chloride used as a rinse). After stirring cold for 30 minutes, the mixture is allowed to stir at ambient temperature for completion of the reaction. The reaction mixture is washed 1× with 1N HCL, dried (Na2SO4) and filtered. Flash chromatography (silica gel, 20% ethyl acetate/hexane as eluant) of the residue obtained gives the title compound (28) (0.33 g) as a colorless oil.

1. washa rinse)
2. stirringto stir at ambient temperature for completion of the reaction
3. washThe reaction mixture is washed 1× with 1N HCL
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customFlash chromatography (silica gel, 20% ethyl acetate/hexane as eluant) of the residue obtained