反应详情

A mixture comprising 5.0 g of α-(4-tert-butylphenyl)-β-hydroxy-β-(2-trifluoromethylphenyl)acrylonitrile, 2.0 g of sodium carbonate and 30 ml of acetone, was heated, and a mixture comprising 2.1 g of methyl chlorothiolformate and 10 ml of acetone, was dropwise added over a period of 10 minutes under reflux. After completion of the dropwise addition, the reaction was carried out for 60 minutes under reflux. The reaction mixture was cooled, and then, an inorganic salt was filtered off. The cake was washed with 20 ml of acetone. Acetone in the filtrate was distilled off, and 50 ml of ISOPAR G (tradename) was added to the residue, followed by heating and dissolution. Then, the solution was left to cool to room temperature. Precipitated crystals were collected by filtration, and the cake was washed with 10 ml of ISOPAR G (tradename) and then dried at 45° C. for 12 hours to obtain 4.8 g of the desired product (isomer ratio 0:100). The HPLC conditions for the analysis of this product were the same as in Preparation Example 5. Further, the NMR spectrum data of this product were the same as the geometrical isomer having a longer retention time of Preparation Example 4.

1. temperaturewas heated
2. temperatureunder reflux
3. additionAfter completion of the dropwise addition
4. temperatureunder reflux
5. temperatureThe reaction mixture was cooled
6. filtrationan inorganic salt was filtered off
7. washThe cake was washed with 20 ml of acetone
8. distillationAcetone in the filtrate was distilled off
9. addition50 ml of ISOPAR G (tradename) was added to the residue
10. temperatureby heating
11. dissolutiondissolution
12. waitThen, the solution was left
13. customPrecipitated crystals
14. filtrationwere collected by filtration
15. washthe cake was washed with 10 ml of ISOPAR G (tradename)
16. customdried at 45° C. for 12 hours