反应详情

温度

0 °C

7.4 g (45 mmol) of CDT was added to a solution of 10.5 g (44.6 mmol) methyl-2-amino-3-(3,4-diethyl-phenyl)-propionate (Intermediate product 48) in 250 mL THF cooled to 0° C. and the resulting mixture was stirred for a further 30 minutes at this temperature. Then 10.9 g (44.6 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one was added, while the reaction solution was kept at this temperature for a further 20 minutes, before being refluxed for 30 minutes. The solvent was eliminated in vacuo, the residue was taken up in sat. sodium bicarbonate solution, exhaustively extracted with ether/EtOAc (1:1) and dried over magnesium sulphate. After removal of the drying agent and solvent the crude product was reacted without any further purification.

1. waitwas kept at this temperature for a further 20 minutes
2. temperaturebefore being refluxed for 30 minutes
3. extractionexhaustively extracted with ether/EtOAc (1:1)
4. dry with materialdried over magnesium sulphate
5. customAfter removal of the drying agent and solvent the crude product
6. customwas reacted without any further purification