反应详情

温度

35 °C

To a methanol (203 g) solution of potassium thioacetate (70.4 g, 0.616 mol, 1.3 equivalent amounts based on the starting material), a mixed solution of a 33 mass % methanol solution (408.5 g, 0.473 mol) of methyl 2-(4-t-butylphenyl)-2-bromoacetate and methanol (270 g) was dropwise added over a period of 1 hour and 20 minutes, followed by stirring at from 30 to 40° C. for 1 hour. Then, the reaction solution was mixed with heptane (674 g) and water (675 g) and stirred for 20 minutes, followed by liquid separation. The solvent was distilled off from the obtained organic layer under reduced pressure at 40° C. until the total amount became 382 g. The obtained solution was cooled to 30° C. over a period of 1 hour, and 0.13 g of seed crystals were added. Then, the solution was stirred for 1 hour and further cooled to −10° C. over a period of 3 hours. Then, the solution was stirred for 1 hour and subjected to filtration, and the obtained crystals were dried to give the desired product (110.7 g, yield: 83.3%).

1. additionwas dropwise added over a period of 1 hour and 20 minutes
2. stirringstirred for 20 minutes
3. customfollowed by liquid separation
4. distillationThe solvent was distilled off from the obtained organic layer under reduced pressure at 40° C. until the total amount
5. temperatureThe obtained solution was cooled to 30° C. over a period of 1 hour
6. addition0.13 g of seed crystals were added
7. stirringThen, the solution was stirred for 1 hour
8. temperaturefurther cooled to −10° C. over a period of 3 hours
9. stirringThen, the solution was stirred for 1 hour
10. filtrationsubjected to filtration
11. customthe obtained crystals were dried