反应详情

Treat a solution of 2-aza-spiro[4.5]decan-1-one (0.50 g, 3.26 mmol) in DMF (8 mL) with 60% sodium hydride (0.20 g, 5.0 mmol) and stir at room temperature for 20 minutes under N2. Cool the reaction to 0° C., treat with 2-bromomethyl-1,3-dichloro-5-benzyloxy-benzene (1.24 g, 3.58 mmol), 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 the reaction with diethyl ether, and then 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 1.23 g (90%) of the titled product. Rf=0.23 (3/1 ethyl acetate/hexanes). MS (m/z): 418 (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. additiondilute
7. washwash with water
8. dry with materialDry the organic layer with Na2SO4
9. customremove the solvent in vacuo
10. customto afford crude product
11. customPurify with a 0 to 100% ethyl acetate in hexanes gradient on silica gel