反应详情

To 10 ml of N,N-dimethylformamide was added dropwise 1.11 g (7.24 mmol) of phosphoryl chloride over 8 minutes with stirring under ice cooling. After the mixture was stirred for 1 hour, 2.67 g (7.23 mmol) of 4-[(3-benzyloxyphenyl) butylamino]butyl acetate dissolved in 4 ml of N,N-dimethylformamide was added dropwise thereto. After stirred for 1 hour, the mixture was gradually heated and stirred at 50° C. for 3 hours and further at 70° C. for 0.5 hours. To this mixture, 20 ml of a 20% sodium acetate solution was added dropwise under cooling in an ice bath. The mixture was stirred for 1 hour and subjected to extraction with ethyl acetate. Washing was performed with a saturated sodium bicarbonate solution and then with a saturated saline solution. Drying over anhydrous sodium sulfate and concentration were performed. The residue was purified by silica gel column chromatography to give 2.14 g of a yellow oily matter (yield: 74.7%).

1. stirringAfter the mixture was stirred for 1 hour
2. additionwas added dropwise
3. stirringAfter stirred for 1 hour
4. temperaturethe mixture was gradually heated
5. stirringstirred at 50° C. for 3 hours and further at 70° C. for 0.5 hours
6. temperatureunder cooling in an ice bath
7. stirringThe mixture was stirred for 1 hour
8. extractionsubjected to extraction with ethyl acetate
9. washWashing
10. dry with materialDrying over anhydrous sodium sulfate and concentration
11. customThe residue was purified by silica gel column chromatography
12. customto give 2.14 g of a yellow oily matter (yield: 74.7%)