反应 #2832

反应方程式

3-nitrobenzoic acid

1-hydroxybenzotriazole

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

morpholine

→

compound ( [13]-(132)-158 )

收率 89.8%

3-nitrobenzoic acid morpholide

收率 89.8%

溶剂

tetrahydrofuran

dichloromethane

chloroform

反应条件

后处理

1. 1
   洗涤The mixture was washed with 1N-HCl aqueous solution, 1N-NaOH aqueous solution
2. 2
   workup.DISTILLATIONdistilled water
3. 3
   干燥The organic layer was dried over anhydrous sodium sulfate
4. 4
   其他The solvent was evaporated under reduced pressure
5. 5
   其他the residue was purified by silica gel column chromatography (Kieselgel 60=160 g, ethyl acetate)

实验过程

In tetrahydrofuran (100 ml) and dichloromethane (100 ml), 3-nitrobenzoic acid (7.58 g) was dissolved. Then 1-hydroxybenzotriazole (6.74 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (9.57 g), and morpholine (9.47 g) were added to the solution. The mixture was stirred at room temperature overnight. After the reaction was completed, chloroform was added to the solution. The mixture was washed with 1N-HCl aqueous solution, 1N-NaOH aqueous solution, and distilled water. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=160 g, ethyl acetate) to obtain the above-captioned compound ([13]-(132)-158) (9.62 g) as white crystals.

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