反应详情

This compound was prepared according to M. E. Flaugh, T. A. Crowell, J. A. Clemens, B. D. Sawyer J. Med. Chem., 1979, 22, pp. 63-68. Acetic anhydride (8.06 g, 79.0 mmol) and NaOAc (1.45 g, 17.7 mmol) were mixed and heated. Two drops of pyridine were added. 2-nitroethanol (6.45 g, 70.8 mmol) was carefully added to the suspension at 30-35° C. during 30 min. Thereafter the mixture was stirred overnight at room temperature. The next morning the mixture contained undissolved NaOAc and a new orange precipitate. The reaction mixture was taken up between CHCl3 and water, washed 1× with water, 1× with brine and dried with MgSO4. Thereafter the solvent was evaporated under reduced pressure at 40° C. The remaining orange oil was co-evaporated first with chloroform and then five times with toluene and finally with chloroform to get the 6.90 g of pure compound.

1. customThis compound was prepared
2. temperatureheated
3. washwashed 1× with water, 1× with brine
4. dry with materialdried with MgSO4
5. customThereafter the solvent was evaporated under reduced pressure at 40° C