反应详情

A solution of 3,3-dimethylacrylic acid (7 g, 70 mmol) and benzyl mercaptan (8.9 mL, 7.5 mmol) in piperidine (70 mL) was heated to reflux for 2 days. Piperidine was then evaporated and the product was partitioned between EtOAc and an aqueous solution of 1N HCl. The organic phase was washed with brine and dried over MgSO4. After evaporation of the solvent the product was distilled with a Kugelrohr apparatus under high vacuum (1 mmHg) to give 15.5 g of the title compound (99% yield).

1. temperatureto reflux for 2 days
2. customPiperidine was then evaporated
3. customthe product was partitioned between EtOAc
4. washThe organic phase was washed with brine
5. dry with materialdried over MgSO4
6. customAfter evaporation of the solvent the product
7. distillationwas distilled with a Kugelrohr apparatus under high vacuum (1 mmHg)