[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[N+:6]([O:9][CH2:10][CH2:11][CH2:12][OH:13])([O-:8])=[O:7].C(N(CC)CC)C>>[C:1]([O:13][CH2:12][CH2:11][CH2:10][O:9][N+:6]([O-:8])=[O:7])(=[O:4])[CH2:2][CH3:3]9.1 mmol Propionyl chloride were dissolved in 10 ml TMBE and cooled to 3° C. 8.25 mmol 3-Nitrooxypropanol and 9.1 mmol triethylamine in 5 ml TMBE were dropped over a period of 5 min at 3 to 6° C. After 2 hours and 30 minutes stirring without cooling the reaction mixture were extracted with 1N HCl, twice with water, washed with brine, dried over Na2SO4 and the solvent was removed in vacuo leaving 1.35 g.
読み込み中…