反应详情

温度

21 °C

To a mixture of 1-hydroxybenzotriazole (30.6 g), 1,2-dimethoxyethane (150 ml), and pyridine (16 g), there was added, while stirring at 21° C., pivaloyl chloride (24.1 g) during 0.75 hr. During the addition, the temperature of the reaction mixture was raised to 34° C. by the heat evolved. The reaction was then heated externally at 88° C. for an additional 0.5 hr. period then cooled, washed with water, and extracted with 1,1,2-trichlorotrifluoroethane. The extract was dried and stripped of solvent and the residue was column chromatographed on neutral alumina in benzene solvent. The product, 1-benzotriazolyl pivalate, was obtained as a brown oil after removal of the benzene solvent. The elemental analysis was as follows:

1. additionwas added
2. additionDuring the addition
3. temperaturethe temperature of the reaction mixture was raised to 34° C. by the heat
4. temperatureThe reaction was then heated externally at 88° C. for an additional 0.5 hr
5. temperatureperiod then cooled
6. washwashed with water
7. extractionextracted with 1,1,2-trichlorotrifluoroethane
8. customThe extract was dried
9. customchromatographed on neutral alumina in benzene solvent