反应详情

The stirred solution of 0.980 g of benzyl 4-(4-hydroxymethylphenyl)-3-[4-(3-methoxypropyl)-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethoxy]piperidine-1-carboxylate and 20 ml of dichloromethane is admixed with 2.12 ml of 1-chloro-N,N,2-trimethylpropenylamine (chlorenamine) in portions over 24 hours. The reaction mixture is poured onto water (100 ml) and extracted with tert-butyl methyl ether (100 ml). The organic phase is washed with brine (50 ml), dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained as a slightly yellowish oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.39 (2:1 EtOAc-heptane); Rt=5.57

1. additionThe reaction mixture is poured onto water (100 ml)
2. extractionextracted with tert-butyl methyl ether (100 ml)
3. washThe organic phase is washed with brine (50 ml)
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated by evaporation