反应详情

温度

24 °C

Triethylamine (0.27 g, 2.75 mmol) was added in one portion to a stirred solution of 1.3 g (2.75 mmol) of (±)-N-(2,6-diisopropylphenyl)-2-(2-dodecyl-2H-tetrazol -5-yl)-2-amino-acetamide (prepared as in Example 10) in 50 mL of THF. To the solution was added in one portion 0.23 g (3.0 mmol) of acetyl chloride. The mixture was stirred at 24° C. for 15 minutes, diluted with 50 mL of ethyl acetate, washed with 50 mL of 1N hydrochloric acid, then with 50 mL of 1N sodium hydroxide, brine, and finally dried over MgSO4. The solution was filtered and concentrated by removing the solvents in vacuo to afford an oil. The oil was further purified by chromatography over silica gel (eluting with 1:1 ethyl acetate/hexane) to provide 0.65 g of (±)-N-(2,6-diisopropylphenyl)-2-(2-dodecyl-2H-tetrazol -5-yl)-2-acetylamino-acetamide;

1. washwashed with 50 mL of 1N hydrochloric acid
2. dry with materialwith 50 mL of 1N sodium hydroxide, brine, and finally dried over MgSO4
3. filtrationThe solution was filtered
4. concentrationconcentrated
5. customby removing the solvents in vacuo
6. customto afford an oil
7. customThe oil was further purified by chromatography over silica gel (eluting with 1:1 ethyl acetate/hexane)