反应详情

温度

50 °C

To a solution of 3-chloro-5-trifluoromethoxybenzyl mesylate (8.2 g, 26.8 mmol; see step (i) above) in DMSO (50 mL) was added sodium cyanide (2.6 g, 53.6 mmol). The resulting heterogeneous solution was warmed to 50° C. and sonicated for 1 hour. The reaction was cooled and partitioned between Et2O and H2O. The organics were washed with H2O (2×) and brine (2×). The combined aqueous phases were extracted with Et2O (1×). The combined organics were dried (Na2SO4), filtered and concentrated under a low heat and partial vacuum to afford the sub-title compound (6.3 g, 100%) as a reddish volatile oil which was used in the next step without further purification.

1. customsonicated for 1 hour
2. temperatureThe reaction was cooled
3. custompartitioned between Et2O and H2O
4. washThe organics were washed with H2O (2×) and brine (2×)
5. extractionThe combined aqueous phases were extracted with Et2O (1×)
6. dry with materialThe combined organics were dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated under
9. temperaturea low heat