反应详情

温度

35 °C

In a reaction vessel, 1.50 kg of the compound of the formula (VI) were initially charged in 14.25 l of isopropanol, and the mixture was heated with stirring to 35° C. 531 g of methyl chloroformate were, at a steady rate, metered in over a period of 30 min, rinsing with 750 ml of isopropanol, and the mixture was stirred at 35° C. for 16 h. The mixture was then heated to 50° C. and 3.85 l of methanol and 606 g of triethylamine were metered in with stirring at 50° C., rinsing with 450 ml of methanol. The mixture was then stirred at 50° C. for 1 h, cooled to RT and stirred at RT for 1 h. The suspended solid was filtered off with suction, washed twice with in each case 3.0 l of isopropanol/methanol (4:1) and once with 3.0 l of isopropanol and sucked dry. The moist product was dried at 50° C. for 1 h and then at 100° C. for 22 h in a vacuum drying cabinet. The weight of the product obtained was 1.793 kg or 103.3% of theory. The product of the formula (VI) contained 6.45% of isopropanol virtually unremovable by drying (partially, an isopropanol solvate was present), and the analytical content was 87.9% by weight (HPLC). Based on this content, the yield was 90.8% of theory.

1. temperaturethe mixture was heated
2. custommetered in over a period of 30 min
3. washrinsing with 750 ml of isopropanol
4. stirringthe mixture was stirred at 35° C. for 16 h
5. temperatureThe mixture was then heated to 50° C.
6. stirringwith stirring at 50° C.
7. washrinsing with 450 ml of methanol
8. stirringThe mixture was then stirred at 50° C. for 1 h
9. temperaturecooled to RT
10. stirringstirred at RT for 1 h
11. filtrationThe suspended solid was filtered off with suction
12. washwashed twice with in each case 3.0 l of isopropanol/methanol (4:1) and once with 3.0 l of isopropanol
13. customsucked dry
14. customThe moist product was dried at 50° C. for 1 h
15. customat 100° C. for 22 h in a vacuum drying cabinet
16. customThe weight of the product obtained
17. dry with materialby drying (partially, an isopropanol solvate