反应详情

0.620 g of 1-azabicyclo[2.2.2]octane-4-carboxylic acid was dissolved in 40 ml of acetonitrile. After adding 3.98 g of N-methyl-N-(trimethylsilyl)trifluoroacetamide, the resulting mixture was stirred for 2 hours. Next, 0.998 g of 8-chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine was added thereto and the resulting mixture was heated under reflux for 4 hours. After distilling off the solvent under reduced pressure, the residue was dissolved in methanol/dichloromethane. After adding diethyl ether, the mixture was filtered and the residue was purified by High-porous gel chromatography (CHP20P, mfd by Mitsubishi Chemical Industries, 75-150μ) (eluted with methanol/water) to thereby give 0.21 g of the title compound as a yellow powder.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 4 hours
3. distillationAfter distilling off the solvent under reduced pressure
4. dissolutionthe residue was dissolved in methanol/dichloromethane
5. additionAfter adding diethyl ether
6. filtrationthe mixture was filtered
7. customthe residue was purified by High-porous gel chromatography (CHP20P, mfd by Mitsubishi Chemical Industries, 75-150μ) (eluted with methanol/water)