反応 #2828

反応方程式

pyridine

methyl 3-aminobenzoate

valeryl chloride

→

methyl 3-valeramidobenzoate

溶媒

water

反応条件

後処理

1. 1
   温度while cooling on ice
2. 2
   抽出The whole was extracted with ethyl acetate
3. 3
   洗浄washed with 5% sodium hydrogencarbonate aqueous solution and water
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   その他The solvent was evaporated
6. 6
   その他the residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1)
7. 7
   その他to obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid

実験手順

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.

出典