反应详情

3 parts of 2-(2-tetrahydrothienyl)-3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one was added to 9.9 parts of oxalic chloride, the mixture was stirred at room temperature for 1.5 hours and concentrated at a temperature below 50° C. The residue was dissolved in 40 parts by volume of benzene and 1.0 part of pyrolidine was added thereto. After stirring at room temperature for 1 hour, the mixture was washed with water, a saturated aqueous sodium hydrogen carbonate solution, and a saturated aqueous sodium chloride solution, in the order listed, and then dried. Benzene was distilled off and the residue was passed through a column containing silica gel using a solvent mixture of chloroform and benzene (2:1) as a spreading agent to obtain 1.1 parts of 3-chloro-2-(2-tetrahydrothienyl)-5,5-dimethyl-2-cyclohexen-1-one as a brown colored oily product.

1. concentrationconcentrated at a temperature below 50° C
2. dissolutionThe residue was dissolved in 40 parts by volume of benzene and 1.0 part of pyrolidine
3. additionwas added
4. stirringAfter stirring at room temperature for 1 hour
5. washthe mixture was washed with water
6. customdried
7. distillationBenzene was distilled off
8. additioncontaining silica gel using
9. additiona solvent mixture of chloroform and benzene (2:1) as a spreading agent