反应详情

温度

110 °C

To a solution of 6-methoxy-1,3,3-trimethyl-1,3-dihydro-indol-2-one (601 mg, 2.93 mmol, example 79) in acetic acid (880 μL) is added hydrobromic acid (48% in H2O) (8.8 mL). The resulting solution is heated to reflux (105°110° C.), stirred 2 hrs, then cooled to room temp and concentrated under reduced pressure. The residue is dissolved in EtOAc and the organic layer washed with water, brine, dried over MgSO4 and concentrated. The residue is purified by triturating with a small volume of ether to give the title compound as an off white solid. MS (ESI) 192 (M+H)+.

1. temperatureThe resulting solution is heated
2. temperaturecooled to room temp
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue is dissolved in EtOAc
5. washthe organic layer washed with water, brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customThe residue is purified
9. customby triturating with a small volume of ether