反应详情

温度

80 °C

A solution of 1.29 g of benzyl 3-hydroxypyrrolidine-1-carboxylate in 80 ml of THF is cooled to 0° C., 0.245 g of 60% NaH in oil is added and then 1.26 g of [(2-bromoethoxy)methyl]benzene and 0.108 g of tetrabutylammonium iodide and it is heated at 80° C. for 3 hours. 0.28 g of NaH and 0.40 g of [(2-bromoethoxy)methyl]benzene are added and it is heated at 80° C. for 2 hours. The reaction mixture is concentrated under vacuum, the residue is extracted with DCM, the organic phase is washed with 0.1M HCl solution, with a saturated solution of NaHCO3, it is dried and the solvent is evaporated under vacuum. The product thus obtained is purified by preparative HPLC and 0.46 g of the expected compound is obtained.

1. concentrationThe reaction mixture is concentrated under vacuum
2. extractionthe residue is extracted with DCM
3. washthe organic phase is washed with 0.1M HCl solution, with a saturated solution of NaHCO3, it
4. customis dried
5. customthe solvent is evaporated under vacuum
6. customThe product thus obtained
7. customis purified by preparative HPLC