反应详情

A solution of ethyl(4-hydroxy-2-methylphenoxy)acetate (intermediate 7, 1.05 g) and 2-(2-thienyl)ethanol (0.64 g) in dry tetrahydrofuran was treated with tri-n-butyl phosphine (1.2 g) and azodicarbonyldimorpholide (1.53 g) and the mixture stirred at ambient temperature for 3 days. The reaction mixture was concentrated and the residue partitioned between ethyl acetate and water. The organic layer was collected, dried over sodium sulfate, concentrated and the residue purified by SPE (Si cartridge) eluting with cyclohexane:ethyl acetate (20:1) to give the title compound as a colourless oil.

1. concentrationThe reaction mixture was concentrated
2. customthe residue partitioned between ethyl acetate and water
3. customThe organic layer was collected
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customthe residue purified by SPE (Si cartridge)
7. washeluting with cyclohexane:ethyl acetate (20:1)