反应详情

温度

110 °C

80.4 g of 1-docosanyl methanesulfonate was added to 207 mL of tetraethylene glycol, and the mixture was heated at 110° C. 40.0 g of t-butoxypotassium was gradually added over 2 hours. The mixture was further stirred for 3 hours, and after cooling, the reaction mixture was poured into 3 L of ice water, to which was then added 2 L of ethyl acetate, the mixture was stirred, and 22.2 g of an insoluble matter was filtered. An ethyl acetate phase was extracted and separated from the filtrate, after concentration under reduced pressure, 0.5 L of acetonitrile was added, and the mixture was stirred under ice cooling for one hour. The reaction mixture was filtered under reduced pressure and washed with 0.2 L of cold acetonitrile to obtain 81.6 g of a white crystal.

1. temperatureafter cooling
2. stirringthe mixture was stirred
3. filtration22.2 g of an insoluble matter was filtered
4. extractionAn ethyl acetate phase was extracted
5. customseparated from the filtrate
6. concentrationafter concentration under reduced pressure, 0.5 L of acetonitrile
7. additionwas added
8. stirringthe mixture was stirred under ice cooling for one hour
9. filtrationThe reaction mixture was filtered under reduced pressure
10. washwashed with 0.2 L of cold acetonitrile