反应 #9749

反应方程式

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

溶剂

tetrahydrofuran

反应条件

后处理

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

实验过程

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.

来源