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 phases were 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 with 99% yield.

1. temperatureto reflux for 2 days
2. customPiperidine was then evaporated
3. customthe product was partitioned between EtOAc
4. washThe organic phases were 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)
8. customto give 15.5 g with 99% yield