反应 #68225

反应方程式

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

溶剂

chloroform

chloroform

反应条件

后处理

1. 1
   workup.ADDITIONwas added at room temperature
2. 2
   其他the solvent was removed under reduced pressure
3. 3
   其他To the residue thus obtained
4. 4
   其他the organic layer was separated
5. 5
   萃取the aqueous layer was extracted with chloroform
6. 6
   洗涤washed with aqueous saturated sodium chloride solution
7. 7
   干燥dried over anhydrous magnesium sulfate
8. 8
   其他the solvent was removed under reduced pressure
9. 9
   其他To the residue thus obtained
10. 10
    过滤the resulting solid was filtered

实验过程

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.

来源