反应详情

To a solution of the hydroxylamine intermediate from Step 4 (1.62 g, 4.7 mmol) in THF (15 mL) there was added 85% trimethylsilyl isocyanate (954 mg, 7.25 mmol). The mixture was stirred at room temperature for 30 minutes. Water (10 mL) was added and stirring was continued for a further 10 minutes. Ethyl acetate was then added, the organic layer was decanted, washed with brine, dried over MgSO4 and evaporated to dryness. The residue was triturated with ether and filtered to afford the pure title product as a yellow solid, mp: 149° C. dec.

1. stirringstirring
2. waitwas continued for a further 10 minutes
3. customthe organic layer was decanted
4. washwashed with brine
5. dry with materialdried over MgSO4
6. customevaporated to dryness
7. customThe residue was triturated with ether
8. filtrationfiltered