反应详情

温度

70 °C

A mixture comprising 5.0 g of α-(4-tert-butylphenyl)-β-hydroxy-β-(2-trifluoromethylphenyl)acrylonitrile, 1.5 g of sodium carbonate and 30 ml of methyl ethyl ketone, was heated to 70° C., and a mixture comprising 2.1 g of methyl chlorothiolformate and 10 ml of methyl ethyl ketone, was dropwise added over a period of 10 minutes. After completion of the dropwise addition, the reaction was carried out for 30 minutes at a temperature of from 70 to 75° C. The reaction mixture was cooled, and then an inorganic salt was filtered off. The cake was washed with 20 ml of methyl ethyl ketone. Methyl ethyl ketone in the filtrate was distilled off, and to the residue, 50 ml of an isoparaffin type hydrocarbon (tradename: ISOPAR G, manufactured by EXXON CHEMICAL) was added, followed by heating for dissolution, and 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 65° C. for 12 hours to obtain 4.9 g of the desired product (isomer ratio 2:98). The HPLC conditions for the analysis of this product were as follows. Further, the NMR spectrum data of this product were the same as in Preparation Example 4.

1. additionAfter completion of the dropwise addition
2. temperatureThe reaction mixture was cooled
3. filtrationan inorganic salt was filtered off
4. washThe cake was washed with 20 ml of methyl ethyl ketone
5. distillationMethyl ethyl ketone in the filtrate was distilled off
6. additionto the residue, 50 ml of an isoparaffin type hydrocarbon (tradename: ISOPAR G, manufactured by EXXON CHEMICAL) was added
7. temperatureby heating for dissolution
8. waitthe solution was left
9. temperatureto cool to room temperature
10. customPrecipitated crystals
11. filtrationwere collected by filtration
12. washthe cake was washed with 10 ml of ISOPAR G (tradename)
13. customdried at 65° C. for 12 hours