تفاعل #68225

معادلة التفاعل

hydrogen chloride ethyl acetate

sodium hydrogen carbonate

tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(2-oxo-4-(pyridin-4-yl)quinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate

trifluoroacetic acid

→

1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-(pyridin-4-yl)quinolin-2(1H)-one hydrochloride

المذيبات

chloroform

chloroform

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added at room temperature
2. 2
   أخرىthe solvent was removed under reduced pressure
3. 3
   أخرىTo the residue thus obtained
4. 4
   أخرىthe organic layer was separated
5. 5
   استخلاصthe aqueous layer was extracted with chloroform
6. 6
   غسيلwashed with aqueous saturated sodium chloride solution
7. 7
   تجفيفdried over anhydrous magnesium sulfate
8. 8
   أخرىthe solvent was removed under reduced pressure
9. 9
   أخرىTo the residue thus obtained
10. 10
    ترشيحthe resulting solid was filtered

الإجراء التجريبي

To 1 mL of a chloroform solution containing 42 mg of tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(2-oxo-4-(pyridin-4-yl)quinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate, 1 mL of trifluoroacetic acid was added at room temperature and stirred for 3.5 hours, thereafter the solvent was removed under reduced pressure. To the residue thus obtained, chloroform and aqueous saturated sodium hydrogen carbonate solution were added, the organic layer was separated and the aqueous layer was extracted with chloroform. The organic layer and extracts were combined, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. To the residue thus obtained, 1 mL of 4 mol/L hydrogen chloride/ethyl acetate was added, the resulting solid was filtered to give 21 mg of (1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-4-(pyridin-4-yl)quinolin-2(1H)-one hydrochloride as a pale yellow solid.

المصدر