반응 #2828

반응 방정식

pyridine

methyl 3-aminobenzoate

valeryl chloride

→

methyl 3-valeramidobenzoate

용매

water

반응 조건

후처리

1. 1
   온도while cooling on ice
2. 2
   추출The whole was extracted with ethyl acetate
3. 3
   세척washed with 5% sodium hydrogencarbonate aqueous solution and water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타The solvent was evaporated
6. 6
   기타the residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1)
7. 7
   기타to obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid

실험 절차

To anhydrous pyridine (120 ml), methyl 3-aminobenzoate (5.00 g) was dissolved, and valeryl chloride (4.13 ml) was added while cooling on ice. The mixture was stirred at room temperature for 4 hours. Distilled water was added to the solution. The whole was extracted with ethyl acetate, washed with 5% sodium hydrogencarbonate aqueous solution and water, and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1) to obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid.

출처