反应详情

温度

45 °C

4′-Bromomethyl-2-cyanobiphenyl (75 g, 0.2757 moles) was added to a mixture of potassium carbonate (95.12 g), DM water (225 ml), ethyl acetate (450 ml) and L-valine methyl ester hydrochloride (55.45 g, 0.330 moles) at 20-30° C. The reaction mixture was heated to 40-50° C. and stirred for 25 h. After completion of the reaction, the ethyl acetate layer was separated at 20-30° C., added DM water (375 ml) and adjusted the pH to 0.8-1.0 with dilute hydrochloric acid at 20-30° C. The aqueous layer was separated and extracted the product in to toluene (430 ml) by adjusting the pH to 8.0-8.5 with 20% w/w aqueous sodium carbonate solution. The toluene layer was washed with DM water (225 ml), concentrated under reduced pressure and dissolved in toluene (450 ml)

1. customAfter completion of the reaction
2. customthe ethyl acetate layer was separated at 20-30° C.
3. additionadded DM water (375 ml)
4. customat 20-30° C
5. customThe aqueous layer was separated
6. extractionextracted the product in to toluene (430 ml)
7. washThe toluene layer was washed with DM water (225 ml)
8. concentrationconcentrated under reduced pressure
9. dissolutiondissolved in toluene (450 ml)