تفاعل #2832

معادلة التفاعل

3-nitrobenzoic acid

1-hydroxybenzotriazole

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

morpholine

→

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

المردود 89.8%

3-nitrobenzoic acid morpholide

المردود 89.8%

المذيبات

tetrahydrofuran

dichloromethane

chloroform

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر