反応 #9749

反応方程式

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

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated
2. 2
   その他the residue partitioned between ethyl acetate and water
3. 3
   その他The organic layer was collected
4. 4
   乾燥dried over sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他the residue purified by SPE (Si cartridge)
7. 7
   洗浄eluting with cyclohexane:ethyl acetate (20:1)

実験手順

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.

出典