反应 #77802

反应方程式

triethylamine

ethyl chlorocarbonate

5-formyl-2-methoxybenzoic acid

4-trifluoromethylbenzylamine

→

5-formyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

收率 78.0%

溶剂

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred further for 3 hours at room temperature
2. 2
   洗涤After washed with water
3. 3
   干燥the reaction mixture was dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
5. 5
   其他The residue obtained
6. 6
   其他was purified by means of column chromatography (silica gel, hexane:ethyl acetate=1:1)
7. 7
   其他recrystallized from a mixed solvent of diethyl ether-ethyl acetate-hexane

实验过程

To a suspension of 1.00 g of 5-formyl-2-methoxybenzoic acid in 50 ml of methylene chloride were added 1.00 ml of triethylamine and 0.60 ml of ethyl chlorocarbonate, and the mixture was stirred for 15 minutes at room temperature. Then, a solution of 1.17 g of 4-trifluoromethylbenzylamine in 10 ml of methylene chloride was added and the mixture was stirred further for 3 hours at room temperature. After washed with water, the reaction mixture was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue obtained was purified by means of column chromatography (silica gel, hexane:ethyl acetate=1:1) and then recrystallized from a mixed solvent of diethyl ether-ethyl acetate-hexane to obtain 1.46 g of 5-formyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as colorless crystals.

来源