反应详情

温度

0 °C

Trifluoromethanesulfonic anhydride (6.04 ml, 35.7 mmol) was added to an ice cooled solution of 1,1-dimethylethyl 9-hydroxy-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (Preparation 62) (6.32 g, 23.82 mmol) in pyridine (100 ml) and stirred at 0° C. for 2 hrs. The pyridine was evaporated and the residue dissolved in EtOAc. Washed with 2M HCl, sat sodium bicarbonate solution, dried over magnesium sulphate and evaporated to give the title compound (9 g) as a yellow oil. MS (ES): C15H18F3NO6S requires 397; found 298 [M+H−100]+.

1. customThe pyridine was evaporated
2. dissolutionthe residue dissolved in EtOAc
3. washWashed with 2M HCl
4. dry with materialdried over magnesium sulphate
5. customevaporated