反应详情

To a solution of the product of Example 8, Step B (75 mg, 0.17 mmol) in 5 mL of toluene was added trimethyltin azide (43 mg, 0.21 mmol, 1.2 eq). The mixture was heated at reflux for 18 hours. Toluene was removed in vacuo and the resultant oil was dissolved in 5 mL of THF and treated with 0.5 mL of 2.5N HCl at 0° C. for 5 minutes. The volatiles were removed in vacuo and the resultant oil was flash chromatographed with 20% of 10/1 methanol/NH4OH mixture in chloroform to yield the titled compound (48.2 mg, 60%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 18 hours
3. customToluene was removed in vacuo
4. dissolutionthe resultant oil was dissolved in 5 mL of THF
5. additiontreated with 0.5 mL of 2.5N HCl at 0° C. for 5 minutes
6. customThe volatiles were removed in vacuo
7. customchromatographed with 20% of 10/1 methanol/NH4OH mixture in chloroform