تفاعل #2468024

معادلة التفاعل

N-cyclopropyl-3-fluoro-4-methyl-5-{3-[1-methyl-1-(tetrahydro-2H-pyran-2-yloxy)ethyl][1,2,4]triazolo[4,3-a]pyridin-7-yl}benzamide

4-methylbenzenesulfonic acid hydrate

→

title compound

المردود 78.0%

N-Cyclopropyl-3-fluoro-5-[3-(1-hydroxy-1-methylethyl)[1,2,4]triazolo[4,3-a]pyridin-7-yl]-4-methylbenzamide

المردود 78.0%

المذيبات

ethyl acetate

methanol

ظروف التفاعل

المعالجة

1. 1
   تركيزthe solvent was concentrated under reduced pressure
2. 2
   أخرىthe oil obtained
3. 3
   غسيلThe organic layer was washed with an aqueous solution of sodium bicarbonate and brine
4. 4
   تجفيفdried over anhydrous sodium sulphate
5. 5
   تركيزconcentrated
6. 6
   workup.ADDITIONThe crude was treated with diethyl ether

الإجراء التجريبي

To a solution of N-cyclopropyl-3-fluoro-4-methyl-5-{3-[1-methyl-1-(tetrahydro-2H-pyran-2-yloxy)ethyl][1,2,4]triazolo[4,3-a]pyridin-7-yl}benzamide (0.065 g, 0.14 mmol) in methanol (1 mL) was added 4-methylbenzenesulfonic acid hydrate (0.010 mg, 0.06 mmol). The reaction mixture was stirred at room temperature for 5 hours, the solvent was concentrated under reduced pressure and the oil obtained was dissolved in ethyl acetate. The organic layer was washed with an aqueous solution of sodium bicarbonate and brine, dried over anhydrous sodium sulphate and concentrated. The crude was treated with diethyl ether to obtain the title compound (78%) as a solid.

المصدر