反应详情

温度

3 °C

16.5 mmol 3-Nitrooxypropanol dissolved in 10 ml TMBE and 18.2 mmol Triethylamine were cooled to 3° C. 18.2 mmol benzoylchloride in 5 ml TMBE were dropped over a period of 7 minutes at 3 to 6° C. After 24 hours and 30 minutes stirring without cooling, the reaction mixture was extracted with sated. NaHCO3, water, 1N HCl, twice with water, washed with brine, dried over Na2SO4 and the solvent was removed in vacuo leaving 3.3 g.

1. temperaturewithout cooling
2. extractionthe reaction mixture was extracted with sated
3. washNaHCO3, water, 1N HCl, twice with water, washed with brine
4. dry with materialdried over Na2SO4
5. customthe solvent was removed in vacuo
6. customleaving 3.3 g