반응 #68061

반응 방정식

tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(7-methoxy-4-((methylamino)carbonyl)-2-oxoquinolin-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)-7-methoxy-N-methyl-2-oxo-1,2-dihydroquinoline-4-carboxamide

수율 70.3%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타The solvent was removed under reduced pressure, chloroform and water
3. 3
   workup.ADDITIONwere added
4. 4
   기타The organic layer was separated
5. 5
   추출the aqueous layer was extracted with chloroform
6. 6
   세척washed with aqueous saturated sodium chloride solution
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   기타the solvent was removed under reduced pressure

실험 절차

To 2 mL of a dichloromethane solution containing 0.15 g of tert-butyl (2,3-dihydro-1,4-benzodioxin-6-ylmethyl)(1-(2-(7-methoxy-4-((methylamino)carbonyl)-2-oxoquinolin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate, 2 mL of trifluoroacetic acid was added and stirred at room temperature for 30 min. The solvent was removed under reduced pressure, chloroform and water were added, and adjusted to pH 11 with 20% aqueous sodium hydroxide solution. 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 give 88 mg of 1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)-7-methoxy-N-methyl-2-oxo-1,2-dihydroquinoline-4-carboxamide as a pale yellow foam.

출처