반응 #532340

반응 방정식

2-amino-4,5-dimethoxybenzonitrile

BuLi

4-isopropyl-1-bromobenzene

water

→

(2-amino-4,5-dimethoxy-phenyl)-(4-isopropyl-phenyl)-methanone

용매

ether THF

ether

반응 조건

후처리

1. 1
   기타at rt
2. 2
   온도After that time the solution is cooled to −5° C.
3. 3
   추출extracted with ethyl acetate
4. 4
   기타The organic layer is dried
5. 5
   기타evaporated
6. 6
   workup.DISSOLUTIONThe crude material is dissolved in 200 ml ether
7. 7
   workup.STIRRINGstirred with 100 ml 2N HCl for one hour
8. 8
   기타After chromatography (DCM/MeOH 15:1) the product is obtained as yellow oil

실험 절차

18.8 ml (30 mmol) of BuLi (1.6 M in hexane) is added dropwise to a cooled (−5° C.) solution of 6 g (30 mmol) 4-isopropyl-1-bromobenzene in 25 ml ether. The reaction mixture is stirred for 15 min at −5° C. and one additional hour at rt. After that time the solution is cooled to −5° C. and a solution 1.8 g (10 mmol) 2-amino-4,5-dimethoxybenzonitrile in 20 ml ether/THF (1:1) is added dropwise. After 30 min the reaction mixture is poured slowly into water and extracted with ethyl acetate. The organic layer is dried and evaporated. The crude material is dissolved in 200 ml ether and stirred with 100 ml 2N HCl for one hour. After chromatography (DCM/MeOH 15:1) the product is obtained as yellow oil.

출처