反应详情

Treat a solution of 3-piperidin-1-yl-pyrrolidin-2-one (0.33 g, 1.96 mmol) in DMF (6 mL) with 60% sodium hydride (0.12 g, 3.00 mmol) and stir at room temperature for 15 minutes under N2. Cool the reaction to 0° C., treat with 5-bromo-2-(bromomethyl)-1,3-dichlorobenzene (0.70 g, 2.19 mmol), stir for 15 minutes at 0° C., warm to room temperature, and stir for 3 hours under N2. Quench the reaction with water and dilute with diethyl ether. Dry the organic layer (Na2SO4), remove the solvent in vacuo to afford crude product, and purify with a 0 to 5% methanol in CH2Cl2 gradient to afford 0.718 g (90%) of the titled product. Rf=0.29 (9/1 CH2Cl2/methanol). ES MS (m/z): 407 (M+).

1. temperatureCool
2. customthe reaction to 0° C.
3. stirringstir for 15 minutes at 0° C.
4. temperaturewarm to room temperature
5. stirringstir for 3 hours under N2
6. customQuench
7. customthe reaction with water
8. dry with materialDry the organic layer (Na2SO4)
9. customremove the solvent in vacuo
10. customto afford crude product
11. custompurify with a 0 to 5% methanol in CH2Cl2 gradient