反应详情

温度

-78 °C

To a stirred solution of 1.98 g (10 mmoles) of ethyl-p-fluorophenoxy acetate (Example 155) in 15 ml of dry toluene, cooled to -78° C., under argon, is added, dropwise over 30 minutes, 8 ml of a 1.4M solution of diisobutylaluminum hydride in toluene (11 mmoles). The mixture is stirred for 2 hours at -78° C., 1 ml of methanol is added, followed by 5 ml of water, dropwise. The gel formed is filtered through Celite and washed with 100 ml of ether, portionwise. The organic phase is separated, washed twice with 25 ml of a saturated brine solution, dried with magnesium sulfate, filtered, and evaporated. The oil obtained is distilled at 71°-73° C. (0.1 mm) to give 600 mg (45%) of the subject product as a colorless liquid.

1. additionis added, dropwise over 30 minutes
2. customThe gel formed
3. filtrationis filtered through Celite
4. washwashed with 100 ml of ether
5. customThe organic phase is separated
6. washwashed twice with 25 ml of a saturated brine solution
7. dry with materialdried with magnesium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe oil obtained
11. distillationis distilled at 71°-73° C. (0.1 mm)