تفاعل #94744

معادلة التفاعل

1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

p-toluenesulfonic acid

ethylene glycol

→

oil

1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone ethylene ketal

المذيبات

cyclohexane

ظروف التفاعل

المعالجة

1. 1
   أخرىflask equipped with a Dean Stark trap
2. 2
   درجة الحرارةto reflux overnight
3. 3
   تركيزconcentrated in vacuo
4. 4
   workup.ADDITIONDil NaHCO3 solution was added to the residue
5. 5
   استخلاصextracted with ethyl acetate
6. 6
   تجفيفdried over anh. MgSO4
7. 7
   ترشيحfiltered
8. 8
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

Into a 1 l r.b. flask equipped with a Dean Stark trap was placed 46.4 g (0.12 m) of 1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone, 1.5 g p-toluenesulfonic acid, 50 mL of ethylene glycol and 300 mL of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with ethyl acetate. The organic layer was backwashed with water, dried over anh. MgSO4, filtered and concentrated under reduced pressure to give 45.3 g of an oil which solidified on drying at room temperature under vacuum.

المصدر