反应详情

To 34.6 g (0.12 mol) of (2,6-difluoro-3,5-dimethoxy-phenyl)-carbamic acid tert-butyl ester, 120 mL of trifluoroacetic acid was added to give a homogeneous solution which was stirred at room temperature for 30 minutes. After 30 min., the reaction mixture was concentrated in vacuo. To the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8. The resulting suspension was extracted twice with diethylether. Combined diethylether layers were washed once with brine, dried over sodium sulfate, filtered and evaporated to give 22 g (97%) of title compound. MS (APCI) (m+1)/z 190.1.

1. customto give a homogeneous solution which
2. waitAfter 30 min.
3. concentrationthe reaction mixture was concentrated in vacuo
4. additionTo the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8
5. extractionThe resulting suspension was extracted twice with diethylether
6. washCombined diethylether layers were washed once with brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated