反应详情

温度

69 °C

To a dry 2-5 mL microwave vial under N2 is added material from Example 116 (120 mg, 0.271 mmol) and anhydrous 1,2-dichloroethane (3 mL). The resulting solution is flushed with N2, treated with trimethylstannanol (60 mg, 0.332 mmol), securely capped and heated in a microwave heating unit at 60-78° C. for 6.5 h. The reaction is diluted with ethyl acetate (75 mL), and the organic layer is washed with 0.5N aqueous HCl (3×15 mL), brine (15 mL), dried over Na2SO4, filtered and evaporated to dryness to give 11 mg (95%) of the title compound as a pale yellow glass that contains 0.5 equivalents of the tin reagent. LC/MS (Condition A): ret. T=3.69 min, (M+Na) 452.

1. customThe resulting solution is flushed with N2
2. customsecurely capped
3. temperatureheated in a microwave
4. washthe organic layer is washed with 0.5N aqueous HCl (3×15 mL), brine (15 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated to dryness