反应详情

Treat a solution of 2-aza-spiro[4.5]decan-1-one (0.138 g, 0.901 mmol) in DMF (5 mL) with 60% sodium hydride (0.054 g, 1.35 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 (0.316 g, 0.991 mmol), and stir for 15 minutes at 0° C. Warm to room temperature and stir for 2 hours under N2. Acidify the reaction with 1 N HCl. Dilute with diethyl ether and wash with water. Dry the organic layer with Na2SO4 and remove the solvent in vacuo to afford crude product. Purify with a 0 to 100% ethyl acetate in hexanes gradient on silica gel to afford 0.258 g (73%) of the titled product. Rf=0.24 (3/1 ethyl acetate/hexanes). MS (m/z): 392 (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 2 hours under N2
6. washwash with water
7. dry with materialDry the organic layer with Na2SO4
8. customremove the solvent in vacuo
9. customto afford crude product
10. customPurify with a 0 to 100% ethyl acetate in hexanes gradient on silica gel