反应详情

2.87 g (19.8 mmol) of 1-chloromethyl-3-fluoro-benzene in 5 ml of dry dimethylformamide were added to a suspension of 4.66 g (19.6 mmol) of [2-(3-hydroxy-phenyl)-ethyl]-carbamic acid tert-butyl ester, 4 g of K2CO3 and 0.3 g of potassium iodide in 50 ml of dry dimethylformamide. The reaction was first stirred at room temperature overnight, then was heated up to 50° C. for 6 hours. After evaporation of the solvent, water was added to the residue and the product was extracted with ethyl acetate. 7 g of crude oil were obtained. Purification by flash chromatography using a mixture of ethyl acetate/hexane (1:9→2:8 gradient) gave 5.9 g (86% yield) of the title product as a colourless oil.

1. temperaturewas heated up to 50° C. for 6 hours
2. customAfter evaporation of the solvent, water
3. additionwas added to the residue
4. extractionthe product was extracted with ethyl acetate
5. custom7 g of crude oil were obtained
6. customPurification by flash chromatography
7. additiona mixture of ethyl acetate/hexane (1:9→2:8 gradient)