反应详情

温度

80 °C

To a solution of 0.65 g of N-methyl o-anisidine in 15 mL of acetonitrile, was added 0.280 g of K2CO3, followed by 0.650 g of 1-(diphenylmethyl)-3-methane sulfonyl azetidine. The reaction mixture was heated at 80° C. for 1 h then at 50° C. overnight. Water was added and the mixture was extracted with ether. The organic phase was dried and the solvent was removed under vacuo. The product was filtered through 100 mL of silica gel, eluting a with 15% ethyl acetate/hexanes then 25% ethyl acetate/hexanes to give 0.200 g of the desired product: mp 91-95° C. MS (ES) m/z (relative intensity): 356 (M++H).

1. customat 50° C.
2. customovernight
3. extractionthe mixture was extracted with ether
4. customThe organic phase was dried
5. customthe solvent was removed under vacuo
6. filtrationThe product was filtered through 100 mL of silica gel
7. washeluting a with 15% ethyl acetate/hexanes