反应详情

A solution of 8.0 g of 5-phenyl-2,4-pentadien-1-ol in 30 ml of dimethylformamide (DMF) was added dropwise over a 30-minute period to a mixture of 1.5 g of sodium hydride and 20 ml of DMF, at 5°. The mixture was stirred for 1 hour at 5°. Then 3.3 g of 1A was added to the stirred mixture at 5° and the resulting mixture was stirred for three hours. The mixture then was poured into ice water and extracted with ether, and the aqueous phase was separated, acidified with acetic acid and extracted with methylene chloride. The methylene chloride extracts were washed with water, dried (MgSO4), and stripped of solvent. The residue was triturated in water and then ether, to give a solid which on recrystallization from ethanol gave 1, as a yellow solid, m.p.: 123°-125°.

1. stirringthe resulting mixture was stirred for three hours
2. extractionextracted with ether
3. customthe aqueous phase was separated
4. extractionextracted with methylene chloride
5. washThe methylene chloride extracts were washed with water
6. dry with materialdried (MgSO4)
7. customThe residue was triturated in water
8. customether, to give a solid which
9. customon recrystallization from ethanol
10. customgave 1