反应详情

To a solution of 5-bromoisoquinoline-N-oxide (4.56 g, 20.4 mmol) in 100 mL CH2Cl2, phosphorus oxychloride (4.17 ml, 44.8 mmol) was added and the mixture heated at 45 C for 4 h. The mixture was allowed to cool and evaporated. Water and ice were added alternating, portion-wise and CH2Cl2 was added to the mixture. The organic layer was made pH 14 with 1 M NaOH, and the organic layer washed with sat. NaHCO3, dried over Na2SO4, filtered and evaporated. The solid was triturated with methanol and the title compound collected as a fluffy off-white solid (3.93 g). MS (ESI pos. ion) m/z: 242 (MH+). Calc'd exact mass for C9H5BrClN: 242.

1. temperaturethe mixture heated at 45 C for 4 h
2. temperatureto cool
3. customevaporated
4. additionWater and ice were added
5. additionportion-wise and CH2Cl2 was added to the mixture
6. washthe organic layer washed with sat. NaHCO3
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated
10. customThe solid was triturated with methanol
11. customthe title compound collected as a fluffy off-white solid (3.93 g)