تفاعل #48501

معادلة التفاعل

WSC

(2S)-3-[(6-Chloronaphthalen-2-yl)sulfony]-2-hydroxypropionic acid

1-(piperidin-4-yl)tetrahydropyrimidin-2(1H)-one

HOBt

→

title compound

1-(1-{(2S)-3-[(6-Chloronaphthalen-2-yl)sulfonyl]-2-hydroxypropanoyl}piperidin-4-yl)tetrahydropyrimidin-2(1H)-one

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONdiluted with an aqueous sodium bicarbonate solution
3. 3
   استخلاصextracted with dichloromethane
4. 4
   غسيلThe extract was washed with an aqueous 5% citric acid solution and saturated saline solution
5. 5
   تجفيفdried over sodium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
7. 7
   أخرىThe residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate/methanol=10/1)

الإجراء التجريبي

(2S)-3-[(6-Chloronaphthalen-2-yl)sulfony]-2-hydroxypropionic acid, 1-(piperidin-4-yl)tetrahydropyrimidin-2(1H)-one, and HOBt (23.0 g) were dissolved in DMF, WSC was added thereto, and the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, diluted with an aqueous sodium bicarbonate solution, and extracted with dichloromethane. The extract was washed with an aqueous 5% citric acid solution and saturated saline solution, and dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate/methanol=10/1) to obtain the title compound as a colorless powder.

المصدر