반응 #40856

반응 방정식

(E)-3-(dimethylamino)-1-phenyl-2-p-tolylprop-2-en-1-one

Compound 113

(E)-3-(dimethylamino)-1-phenyl-2-p-tolylprop-2-en-1-one

cyanoacetamide

MeOH

NaH

→

title compound

2-Hydroxy-6-phenyl-5-p-tolylnicotinonitrile

용매

DMF

DMF

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타The reaction was quenched with water
3. 3
   추출extracted with ethyl acetate
4. 4
   세척The organic layer was washed with water and brine
5. 5
   건조dried over MgSO4
6. 6
   농축concentrated in vacuo
7. 7
   기타The solid residue was triturated with diethyl ether
8. 8
   여과filtered
9. 9
   기타dried under high vacuum

실험 절차

A solution of (E)-3-(dimethylamino)-1-phenyl-2-p-tolylprop-2-en-1-one (Compound 113, 500 mg, 1.9 mmol), cyanoacetamide (175 mg, 2.1 mmol) and MeOH (0.2 ml, 2.2 mmol) in DMF (4 ml) was cannulated into a suspension of NaH (119 mg, 4.7 mmol, 95% in mineral oil) in DMF (2 ml) at room temperature. After the addition was completed, the reaction was heated to 95° C. for 2 hours. The reaction was quenched with water and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over MgSO4, concentrated in vacuo. The solid residue was triturated with diethyl ether, filtered and dried under high vacuum to yield the title compound as a white solid.

출처