تفاعل #92746

معادلة التفاعل

8-(cyclohexylmethoxy)-2-methyl-N-[(3S)-piperidin-3-yl]imidazo[1,2-a]pyridine-3-carboxamide dihydrochloride

pyridine

sulfamide

water

→

N-[(3S)-1-(aminosulfonyl)piperidin-3-yl]-8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridine-3-carboxamide hydrochloride

المردود 68.9%

المذيبات

chloroform

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةby heating
2. 2
   درجة الحرارةto reflux for 4 hours
3. 3
   أخرىAfter leaving
4. 4
   أخرىa layer separation operation
5. 5
   تجفيفThe organic layer was dried over anhydrous sodium sulfate
6. 6
   أخرىthe solvent was evaporated under reduced pressure
7. 7
   أخرىthe obtained residue was purified by silica gel column chromatography
8. 8
   workup.ADDITION120 μl of a 4 M hydrogen chloride/ethyl acetate solution was added
9. 9
   ترشيحThe resulting solid was collected by filtration
10. 10
    أخرىdried

الإجراء التجريبي

To 200 mg of 8-(cyclohexylmethoxy)-2-methyl-N-[(3S)-piperidin-3-yl]imidazo[1,2-a]pyridine-3-carboxamide dihydrochloride were added 5 ml of pyridine and 217 mg of sulfamide, followed by heating to reflux for 4 hours. After leaving to be cooled at room temperature, to the reaction mixture were added water and chloroform to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography. The obtained solid was suspended in ethyl acetate, and 120 μl of a 4 M hydrogen chloride/ethyl acetate solution was added thereto. The resulting solid was collected by filtration and dried to obtain 151 mg of N-[(3S)-1-(aminosulfonyl)piperidin-3-yl]-8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridine-3-carboxamide hydrochloride.

المصدر