反应详情

37 g of tert-butanol and then 26 ml of pyridine are added to 39.04 g of p-toluoyl chloride and the reaction mixture is refluxed for 3 hours. After cooling, it is poured into water, extracted with AcOEt, washed with a 1N solution of HCl and then with a 5% solution of sodium hydrogencarbonate, dried over sodium sulfate and evaporated under vacuum. The residue is chromatographed on silica using hexane and then a hexane/DCM mixture (80/20; v/v) as the eluent to give 38.9 g of the expected product, which is used as such in the next step.

1. temperaturethe reaction mixture is refluxed for 3 hours
2. temperatureAfter cooling
3. extractionextracted with AcOEt
4. washwashed with a 1N solution of HCl
5. dry with materialwith a 5% solution of sodium hydrogencarbonate, dried over sodium sulfate
6. customevaporated under vacuum
7. customThe residue is chromatographed on silica