反応 #833525

反応方程式

Acrylic acid chloride

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

N,N-dimethylaniline

dioxane

→

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

収率 88.5%

溶媒

heptane

ethyl acetate

water

toluene

反応条件

後処理

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

実験手順

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.

出典