反应详情

To conc. sulfuric acid (10 ml) was added a solution of 2-methyl-1-phenylpropan-2-ol (7.0 g) and acetonitrile (1.62 ml) in benzene (7.0 ml) dropwise and the mixture was stirred for 24 hours at room temperature. The mixture was neutralized by adding to a mixture of ice and a saturated aqueous solution of sodium bicarbonate dropwise, and it was extracted with ethyl acetate twice. The extract was dried over anhydrous magnesium sulfate and was concentrated under reduced pressure. The residue was dissolved in ether and was extracted with 1N hydrochloric acid and 2N hydrochloric acid. The extract was washed with ether and to the mixture was added 5N aqueous solution of sodium hydroxide and was extracted with ether twice. The extract was washed with water and a saturated aqueous solution of sodium chloride successively, and dried over anhydrous magnesium sulfate and was concentrated under reduced pressure to give the title compound (2.53 g) having the following physical data.

1. additionby adding to a mixture of ice
2. extractiona saturated aqueous solution of sodium bicarbonate dropwise, and it was extracted with ethyl acetate twice
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. concentrationwas concentrated under reduced pressure
5. dissolutionThe residue was dissolved in ether
6. extractionwas extracted with 1N hydrochloric acid and 2N hydrochloric acid
7. washThe extract was washed with ether and to the mixture
8. additionwas added 5N aqueous solution of sodium hydroxide
9. extractionwas extracted with ether twice
10. washThe extract was washed with water
11. dry with materiala saturated aqueous solution of sodium chloride successively, and dried over anhydrous magnesium sulfate
12. concentrationwas concentrated under reduced pressure