反应详情

温度

-78 °C

The product from Example 9 (0.490 g) was dissolved in 25 ml methylene chloride and cooled to -78° C. To the reaction was added 0.69 ml BBr3. The reaction was warmed to 0° C. for 4 h and then cooled to -78° C. The reaction was quenched by the addition of 5 ml methanol and the solvent was evaporated. The resulting solid was recrystallized from ethanol and ether to yield 0.470 g white solid, mp: 187-9° C. NMR (d6DMSO) δ 0.88 (t, 3H), 1.65 (m, 2H), 2.60-4.10 (m, 10H), 6.65 (d, 1H), 6.70 (d, 1H), 7.05 (t, 1H).

1. temperatureThe reaction was warmed to 0° C. for 4 h
2. temperaturecooled to -78° C
3. customThe reaction was quenched by the addition of 5 ml methanol
4. customthe solvent was evaporated
5. customThe resulting solid was recrystallized from ethanol and ether