反应详情

温度

135 °C

A reaction mixture of 4-bromo-6,7-dihydro-5H-isoquinolin-8-one (intermediate B-11 [C], 5.0 g, 22 mmol), 2,2-dimethyl-propane-1,3-diol (2.8 g, 26.5 mmol) and toluene-4-sulfonic acid (85 mg, 0.44 mmol) in toluene (100 mL) was heated at 135° C. for 12 hours. After cooling to room temperature, it was concentrated under reduced pressure to give a residue which was extracted between EtOAc and water. The organic layer was washed with brine, dried over anhy. Na2SO4, filtered, and concentrated in vacuo to give a crude product (6.1 g, 88.9%) as a light yellow solid. MS: 312.2 & 314.2 (M+H+).

1. temperatureAfter cooling to room temperature
2. concentrationit was concentrated under reduced pressure
3. customto give a residue which
4. extractionwas extracted between EtOAc and water
5. washThe organic layer was washed with brine
6. customdried over anhy
7. filtrationNa2SO4, filtered
8. concentrationconcentrated in vacuo