تفاعل #73766

معادلة التفاعل

3-(4-bromo-phenyl)-3-(4-chloro-phenyl)-2-cyano-propionic acid ethyl ester

acetic acid

sulfuric acid

→

desired product

المردود 50.0%

3-(4-Bromo-phenyl)-3-(4-chloro-phenyl)-propionic acid

المردود 50.0%

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwere refluxed for 2 hours
2. 2
   أخرىReaction mixture
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   أخرىThe organic layer was separated
5. 5
   تجفيفdried (MgSO4)
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated
8. 8
   أخرىthe crude product was purified over flash silica chromatography
9. 9
   غسيلeluting with ethyl acetate/petroleum ether (1:1)

الإجراء التجريبي

A mixture of 3-(4-bromo-phenyl)-3-(4-chloro-phenyl)-2-cyano-propionic acid ethyl ester (1.91, 4.87 mmol), acetic acid (10 ml), concentrated sulfuric acid (5 ml) and water (5 ml) were refluxed for 2 hours. Reaction mixture was poured into iced water and extracted with ethyl acetate. The organic layer was separated, dried (MgSO4), filtered and concentrated, the crude product was purified over flash silica chromatography eluting with ethyl acetate/petroleum ether (1:1) to afford the desired product (0.82 g, 50% yield). LC/MS: (PS-A2) Rt 3.39 [M+H]+ 338.86.

المصدر