反応 #2830

反応方程式

water

4-methoxycarbonylbenzaldehyde

compound ( [5]-(55)-75 )

3-amino-4-hexylbenzoic acid morpholide

→

4-hexyl-3-[(4-methoxycarbonylphenyl)methyl]aminobenzoic acid morpholide

溶媒

acetic acid

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture was stirred at room temperature for 30 minutes
2. 2
   抽出The solution was extracted with ethyl acetate
3. 3
   洗浄washed with distilled water
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   その他The solvent was evaporated under reduced pressure
6. 6
   その他the residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1)
7. 7
   その他to obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid

実験手順

The compound ([5]-(55)-75) (600 mg) prepared in Example 63 was dissolved in acetic acid (6.0 ml). Then, 4-methoxycarbonylbenzaldehyde (373 mg) was added. The mixture was stirred at room temperature for 4 hours. Then, boranediethylamine complex (146 mg) was added to the solution. The mixture was stirred at room temperature for 30 minutes. After the reaction was completed, water was added to the solution. The solution was extracted with ethyl acetate, washed with distilled water, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1) to obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid.

出典