반응 #4666

반응 방정식

ethyl orthoformate

ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate

cyclopropylamine

→

crystals

수율 36.1%

ethyl 3-cyclopropylamino-2-(2,5-difluoro-4-pyrrol-1-ylbenzoyl)acrylate

수율 36.1%

용매

acetic anhydride

반응 조건

후처리

1. 1
   온도the mixture is refluxed for 3 hours
2. 2
   기타It is evaporated to dryness
3. 3
   workup.DISSOLUTIONthe residue is dissolved in 10 ml of ethanol
4. 4
   기타It is evaporated to dryness
5. 5
   추출the oily residue is extracted with 3×30 ml of boiling hexane
6. 6
   농축The hexane fractions are concentrated to 20 ml
7. 7
   workup.WAITleft for 12 hours at 5° C.

실험 절차

1 g (0.0068 mol) of ethyl orthoformate is added to a solution of 1.1 g (0.00315 mol) of ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate in 3 ml of acetic anhydride and the mixture is refluxed for 3 hours. It is evaporated to dryness, the residue is dissolved in 10 ml of ethanol, 0.3 ml (0.0034 mol) of cyclopropylamine is added and the mixture is left at room temperature for 1 hour. It is evaporated to dryness and the oily residue is extracted with 3×30 ml of boiling hexane. The hexane fractions are concentrated to 20 ml and left for 12 hours at 5° C. to give 0.41 g of crystals melting at 90°-2° C.

출처