تفاعل #9749

معادلة التفاعل

ethyl(4-hydroxy-2-methylphenoxy)acetate

intermediate 7

ethyl(4-hydroxy-2-methylphenoxy)acetate

2-(2-thienyl)ethanol

tri-n-butyl phosphine

→

title compound

ethyl[2-methyl-4-(2-thien-2-ylethoxy)phenoxy]acetate

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated
2. 2
   أخرىthe residue partitioned between ethyl acetate and water
3. 3
   أخرىThe organic layer was collected
4. 4
   تجفيفdried over sodium sulfate
5. 5
   تركيزconcentrated
6. 6
   أخرىthe residue purified by SPE (Si cartridge)
7. 7
   غسيلeluting with cyclohexane:ethyl acetate (20:1)

الإجراء التجريبي

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.

المصدر