反应详情

To 20 mL of an N,N-dimethylformamide solution containing 0.57 g of tert-butyl (7-chloro-3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazin-6-ylmethyl)(1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate, 0.04 g of 60% sodium hydride was added, and stirred at room temperature for 1 hour. 0.24 g of methyl iodide was added, and stirred at room temperature for 2 hours. To the reaction mixture, water, ethyl acetate and toluene were added. The organic layer was separated, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [Silica Gel; Kanto Chemical Co., Inc., Silica Gel 60N, eluent; chloroform:methanol=30:1] to give 0.23 g of tert-butyl (7-chloro-4-methyl-3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazin-6-ylmethyl)(1-(2-(7-methoxy-2-oxoquinoxalin-1(2H)-yl)ethyl)piperidin-4-yl)carbamate as a pale brown foam.

1. additionwas added
2. stirringstirred at room temperature for 2 hours
3. customThe organic layer was separated
4. washwashed with aqueous saturated sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was removed under reduced pressure
7. customThe residue thus obtained
8. customwas purified by silica gel column chromatography [Silica Gel; Kanto Chemical Co., Inc., Silica Gel 60N, eluent; chloroform:methanol=30:1]