تفاعل #306943

معادلة التفاعل

NH4Cl

1,2-dichloro-4-fluoro-5-nitrobenzene

methyl 4-chlorophenylacetate

NaH

→

brown oil

Methyl (4-chlorophenyl)(4,5-dichloro-2-nitrophenyl)acetate

المذيبات

DMF

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىThe mixture is reacted for 2 hours
2. 2
   أخرىto return to room temperature
3. 3
   workup.ADDITIONis added
4. 4
   استخلاصthe mixture is extracted with ethyl acetate
5. 5
   أخرىThe organic phase is dried
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated

الإجراء التجريبي

A solution of 5 g of 1,2-dichloro-4-fluoro-5-nitrobenzene and 4.4 g of methyl 4-chlorophenylacetate in 70 ml of DMF is added, under a stream of nitrogen, to a suspension at −10° C. of 2.85 g of 60% NaH in 45 ml of DMF, and the temperature is maintained at −5° C. The mixture is reacted for 2 hours, while allowing the temperature to return to room temperature. The resulting mixture is poured onto ice, aqueous 10% NH4Cl solution is added and the mixture is extracted with ethyl acetate. The organic phase is dried, filtered and concentrated. 30 g of a brown oil are obtained, and are purified on a column with hexane and then with a 95/5 hexane/EtOAc mixture to give 3.18 g of oil.

المصدر