Reacción #833525

Ecuación de reacción

Acrylic acid chloride

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

N,N-dimethylaniline

dioxane

→

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

Rendimiento 88.5%

Disolventes

heptane

ethyl acetate

water

toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   LavadoThe ethyl acetate layer was washed with water
2. 2
   Secadodried over anhydrous magnesium sulfate
3. 3
   OtroThe solvent was removed by distillation from the ethyl acetate layer
4. 4
   Otroto obtain solids
5. 5
   Otrore-precipitated

Procedimiento

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.

Fuente