反应详情

To 5 mL of an ethanol suspension containing 0.15 g of methyl 1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)-4-oxopiperidine-2-carboxylate, 0.16 g of ammonium acetate and 0.20 g of molecular sieves 3A were added at room temperature. After the mixture was stirred for 2 hours and 55 min at room temperature, 21 mg of sodium cyanoborohydride was added, and stirred for 1 hour and 40 min. To the reaction mixture, aqueous saturated sodium hydrogen carbonate solution and chloroform 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 give 0.11 g of methyl 4-amino-1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)piperidine-2-carboxylate as a brown foam. (2) According to a procedure similar to Example 179, methyl 4-((3-fluoro-4-methylbenzyl)amino-1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)piperidine-2-carboxylate was obtained from methyl 4-amino-1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)piperidine-2-carboxylate.

1. additionwere added at room temperature
2. stirringstirred for 1 hour and 40 min
3. customthe organic layer was separated
4. extractionthe aqueous layer was extracted with chloroform
5. washwashed with aqueous saturated sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was removed under reduced pressure