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With 1H-imidazole; dmap In dichloromethane at 0 - 20℃; for 25h; Inert atmosphere;
13 Example 13: Synthesis of Compound 17
To a suspension of 14 (0.980 g, 3.77 mmol) in anhydrous CH2CI2 (37.7 mL) was sequentially added imidazole (0.769 g, 11.30 mmol), DMAP (0.046 g, 0.377 mmol) and TBS Triflate (2.162 mL, 9.42 mmol) at 0 °C under argon. The resulting reaction was stirred at 0 °C for 1 hr. The reaction mixture was then warmed up to r.t. and stirred for 24 hrs. The reaction mixture was washed with H2O, brine and dried over a2S04. After removal of the solvent, the obtained colorless residue was loaded on an ISCO column (40g silica gel). Fractions containing product were collected and condensed on rotavap to give a colorless residue, which turned into a white foam under high vacuum to provide 17 (1.8303 g, 99 % yield).
99%
With 1H-imidazole; dmap In dichloromethane at 0 - 20℃; for 25h; Inert atmosphere;
13
To a suspension of 14 (0.980 g, 3.77 mmol) in anhydrous CH2CI2 (37.7 mL) was sequentially added imidazole (0.769 g, 11.30 mmol), DMAP (0.046 g, 0.377 mmol) and TBS Triflate (2.162 mL, 9.42 mmol) at 0 °C under argon. The resulting reaction was stirred at 0 °C for 1 hr. The reaction mixture was then warmed up to r.t. and stirred for 24 hrs. The reaction mixture was washed with H2O, brine and dried over Na2S04. After removal of the solvent, the obtained colorless residue was loaded on an ISCO column (40g silica gel). Fractions containing product were collected and condensed on rotavap to give a colorless residue, which turned into a white foam under high vacuum to provide 17 (1.8303 g, 99 % yield).
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