反应详情

A solution of 400 g. (2.04 moles) of a mixture of 2-(5-hydroxypentyl)cyclopentanone and 2-(5-acetoxypentyl)cyclopentanone (Example 55) and 4.0 g. of p-toluenesulfonic acid monohydrate in 1 l. of acetic anhydride is refluxed at a rate to maintain a steady distillation of acetic acid from the reaction through a helix-packed fractionation column. The reaction is continued with the addition of acetic anhydride to maintain a constant volume until complete conversion of starting materials to product is evident. The mixture is cooled and partitioned between 2 l. of hexane and 3 l. of cold water containing solid sodium bicarbonate to maintain a neutral pH. The organic phase is washed with saturated brine. dried (MgSO4), and evaporated to yield 452 g. of an oil.

1. temperatureto maintain
2. distillationa steady distillation of acetic acid
3. customfrom the reaction through a helix-packed fractionation column
4. temperatureto maintain a constant volume until complete conversion of starting materials to product
5. temperatureThe mixture is cooled
6. custompartitioned between 2 l
7. temperatureof cold water containing solid sodium bicarbonate to maintain a neutral pH
8. washThe organic phase is washed with saturated brine
9. dry with materialdried (MgSO4)
10. customevaporated
11. customto yield 452 g