反应详情

POCl3 (5.8 g, 37.7 mmol) was added to 20 ml of DMF in an ice bath. After 40 minutes, 2,2-dimethylpropionic acid 2-[(3-methoxyphenyl)methylamino]ethyl ester (10 g, 37.7 mmol) dissolved in DMF (10 ml) was added dropwise. After the mixture was stirred for 16 hours, an aqueous sodium acetate solution (20%, 100 ml) was added dropwise thereto and the oily matter was subjected to extraction with ethyl acetate. Washing was performed with a saturated aqueous NaHCO3 solution (100 ml) and then with a saturated saline solution (100 ml). After drying over Na2SO4 and concentration, the residue was purified by silica gel chromatography to give a light yellow crystal (yield: 8.7 g (78.9%)).

1. additionwas added dropwise
2. extractionthe oily matter was subjected to extraction with ethyl acetate
3. washWashing
4. dry with materialAfter drying over Na2SO4 and concentration
5. customthe residue was purified by silica gel chromatography
6. customto give a light yellow crystal (yield: 8.7 g (78.9%))