反应 #833525

反应方程式

Acrylic acid chloride

(4-(6-hydroxyhexyloxy)phenyl)propionic acid

N,N-dimethylaniline

dioxane

→

(4-(6-acryloyloxyhexyloxy)phenyl)propionic acid

收率 88.5%

溶剂

heptane

ethyl acetate

water

toluene

反应条件

后处理

1. 1
   洗涤The ethyl acetate layer was washed with water
2. 2
   干燥dried over anhydrous magnesium sulfate
3. 3
   其他The solvent was removed by distillation from the ethyl acetate layer
4. 4
   其他to obtain solids
5. 5
   其他re-precipitated

实验过程

Acrylic acid chloride (74.3 g) was dropped for 10 minutes to a mixture of (4-(6-hydroxyhexyloxy)phenyl)propionic acid (200 g), N,N-dimethylaniline (100 g), BHT (0.3 g), and dioxane (1,000 mL). After stirring at 60° C. for 5 hours, the reaction mixture was poured into water and stirred with addition of ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed by distillation from the ethyl acetate layer to obtain solids. The solids were dissolved in toluene and poured into plenty of heptane and re-precipitated to obtain (4-(6-acryloyloxyhexyloxy)phenyl)propionic acid (AK2: 213 g). Melting point: 64° C. to 68° C.

来源