反应详情

There are mixed 14.1 grams (0.05 mole) of the acid from step (a), 0.1 grams triethylamine hydrochloride and 150 milliliters chloroform, followed by stirring and heating to reflux. Then 6.5 grams (0.055 mole) thionyl chloride was slowly added, dropwise. After the addition was complete, the reaction mass was heated under reflux until evolution of HCl had ceased (about 30 minutes). The reaction mixture was cooled to room temperature, and the solvent was removed by vacuum distillation yielding 100 grams (66.7% of theoretical yield) of 2-(3-trifluoromethylphenoxy) nicotinoyl chloride.

1. temperatureheating to reflux
2. additionAfter the addition
3. temperaturethe reaction mass was heated
4. custom(about 30 minutes)
5. customthe solvent was removed by vacuum distillation