반응 #833525
ord-dc8752a737e04cf8b0d74078c20211cf
반응 방정식
Acrylic acid chloride
(4-(6-hydroxyhexyloxy)phenyl)propionic acid
N,N-dimethylaniline
dioxane
→
(4-(6-acryloyloxyhexyloxy)phenyl)propionic acid
수율 88.5%
반응 조건
온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1세척The ethyl acetate layer was washed with water
- 2건조dried over anhydrous magnesium sulfate
- 3기타The solvent was removed by distillation from the ethyl acetate layer
- 4기타to obtain solids
- 5기타re-precipitated
실험 절차
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.