تفاعل #48513

معادلة التفاعل

WSC

[3-{1-[(benzyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acid

methylamine

HOBt

→

title compound

المردود 100.5%

Benzyl 4-[3-(methylcarbonylmethyl)-2-oxotetrahydropyrimidin-1(2H)-yl]piperidin-1-carboxylate

المردود 100.5%

المذيبات

THF

THF dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONThe solvent were distilled off under reduced pressure
2. 2
   workup.ADDITIONthe residue was diluted with ethyl acetate
3. 3
   غسيلThe mixture was washed with an aqueous saturated sodium bicarbonate solution and saturated saline solution
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   تركيزconcentrated under reduced pressure
6. 6
   أخرىThe residue was purified with basic silica gel column chromatography (ethyl acetate)

الإجراء التجريبي

WSC (0.39 g) was added to a solution of [3-{1-[(benzyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acid (0.70 g) obtained in Example 36a), a solution of methylamine in THF (1.85 mL) and HOBt (0.31 g) in THF/dichloromethane (1/1, 30 mL) and the mixture was stirred at room temperature overnight. The solvent were distilled off under reduced pressure, and the residue was diluted with ethyl acetate. The mixture was washed with an aqueous saturated sodium bicarbonate solution and saturated saline solution, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified with basic silica gel column chromatography (ethyl acetate) to obtain the title compound (0.70 g, 97%) as a white powder.

المصدر