反应详情

To a stirred suspension of 14-2 (0.4 g, 1.1 mMol) in anhydrous THF (15 mL) was added 3 mL of concentrated NH4OH. The solution was then treated with iodine (0.4 g, 1.6 mMol) followed by stirring at room temperature overnight. The reaction was quenched with saturated sodium thiosulfate solution (20 mL) and the product was extracted into ethyl acetate three times. The combined organic layers were washed with brine, dried with Na2SO4, filtered and concentrated in vacuo to yield 15-1 as a tan solid. Mass (M+1) calculated: 378.135 observed: 378.1345

1. customThe reaction was quenched with saturated sodium thiosulfate solution (20 mL)
2. extractionthe product was extracted into ethyl acetate three times
3. washThe combined organic layers were washed with brine
4. dry with materialdried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo