反应详情

To a cooled solution of KHMDS (0.5M in toluene, 50 ml, 25 mmol) at 0° C. in dry tetrahydrofuran (70 ml) under nitrogen is added freshly prepared neat (2-trifluoromethyl-benzyl)-phosphonic acid diethyl ester (5.7 ml, 25 mmol, 1 equiv.). The reaction is warmed to room temperature over 1 hour and then racemic (4-benzyl-morpholin-2-yl)-phenyl-methanone (7 g, 25 mmol in 25 ml of dry tetrahydrofuran) is added dropwise. The reaction is left at room temperature and stirred for 2 hours. At the end of this time the reaction solvent is removed under reduced vacuum and replaced with diethyl ether prior to quenching with water. After extraction with diethyl ether and drying (MgSO4) the solvent is again removed under reduced pressure. The resulting residue is purified by column chromatography on silica gel to yield a colourless oil (6.5 g, 61%).

1. waitThe reaction is left at room temperature
2. customAt the end of this time the reaction solvent is removed under reduced vacuum
3. customto quenching with water
4. extractionAfter extraction with diethyl ether
5. dry with materialdrying (MgSO4) the solvent
6. customis again removed under reduced pressure
7. customThe resulting residue is purified by column chromatography on silica gel