反応 #1253189

反応方程式

diethyl azodicarboxylate

triphenylphosphine

4′-hydroxyl-4-biphenylcarboxylic acid

4-hydroxybutyl acrylate

→

4′-hydroxy-biphenyl-4-carboxylic acid 4-acryloylbutyl ester

収率 66.6%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他overnight
2. 2
   その他at room temperature
3. 3
   濃縮The mixture is then concentrated
4. 4
   その他the residue is purified by chromatography on silica gel

実験手順

5.24 g (20 mmol) of triphenylphosphine (TPP) are added at 0° C. to a solution of 4.28 g (20 mmol) of 4′-hydroxyl-4-biphenylcarboxylic acid and 2.88 g (29 mmol) of 4-hydroxybutyl acrylate in 100 ml of tetrahydrofuran (THF) and then, at the same temperature, 3.50 g (20 mmol) of diethyl azodicarboxylate (DEAD) are added dropwise thereto. The mixture is stirred for one hour at 0° C. and then overnight at room temperature. The mixture is then concentrated and the residue is purified by chromatography on silica gel using cyclohexane/ethyl acetate 2:1 to obtain 4.32 g of 4′-hydroxy-biphenyl-4-carboxylic acid 4-acryloylbutyl ester.

出典