تفاعل #71798

معادلة التفاعل

Example ( 56d )

2-[(3S,4R)-4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-4-methyl-1,3-thiazole-5-carboxylic acid

hydrochloric acid

sodium hydroxide

→

title compound

المردود 100.5%

4-Chloro-5-ethyl-N-[(3S,4R)-3-methoxy-1-(5-methyl-1,3-thiazol-2-yl)piperidin-4-yl]-1H-imidazole-2-carboxamide

المردود 100.5%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   استخلاصfollowed by extraction with ethyl acetate
2. 2
   غسيلThen, the organic layer was washed with brine
3. 3
   تجفيفdried over anhydrous sodium sulfate
4. 4
   تركيزconcentration under reduced pressure
5. 5
   أخرىthe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=1/1, ethyl acetate)

الإجراء التجريبي

2-[(3S,4R)-4-{[(4-Chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-4-methyl-1,3-thiazole-5-carboxylic acid obtained by the method described in Example (56d) (15 mg, 0.035 mmol) was dissolved in THF (3 mL). 1 N hydrochloric acid (1 mL) was added, and the mixture was stirred at 60° C. for 40 minutes. A 1 N aqueous sodium hydroxide solution was added to the reaction solution, followed by extraction with ethyl acetate. Then, the organic layer was washed with brine and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=1/1, ethyl acetate) to obtain 13.5 mg of the title compound as a white solid (100%).

المصدر