反应详情

温度

20 °C

15.00 kg (52.22 mol) 1-[2-hydroxy-3-nitro-5-(phenylmethoxy)-phenyl]-ethanone 4a, 0.165 kg platinum (IV) oxide and 45 l 2-methyltetrahydrofuran are hydrogenated at 3 bar hydrogen pressure and an internal temperature of 25° C. until no further hydrogen uptake is discernible. The catalyst is filtered off and washed with 20 l of 2-methyltetrahydrofuran. 23.09 kg (167.09 mol) potassium carbonate are placed in another reactor, and the reaction mixture from the first reactor is added. It is rinsed with 22 l of 2-methyltetrahydrofuran. Then within 30 minutes 9.44 kg (83.55 mol) chloroacetyl chloride are metered into the suspension. After 2.5 hours reaction time at 65° C., 101 l water are added. The aqueous phase is separated off at 55° C. Then 34 l 2-methyltetrahydrofuran are distilled off from the organic phase in vacuo. After heating to reflux temperature, 180 l methylcyclohexane are metered in within 30 minutes at reflux temperature. The suspension obtained is cooled to 20° C. and stirred for another 1 hour at this temperature to complete the crystallisation. Then the precipitate is removed by centrifuging, washed with 113 l methylcyclohexane and dried at 50° C.

1. customan internal temperature of 25° C.
2. filtrationThe catalyst is filtered off
3. washwashed with 20 l of 2-methyltetrahydrofuran
4. additionthe reaction mixture from the first reactor is added
5. washIt is rinsed with 22 l of 2-methyltetrahydrofuran
6. customAfter 2.5 hours reaction time at 65° C.
7. customThe aqueous phase is separated off at 55° C
8. distillationThen 34 l 2-methyltetrahydrofuran are distilled off from the organic phase in vacuo
9. temperatureAfter heating
10. temperatureto reflux temperature, 180 l methylcyclohexane
11. customare metered in within 30 minutes
12. temperatureat reflux temperature
13. customThe suspension obtained
14. customthe crystallisation
15. customThen the precipitate is removed by centrifuging
16. washwashed with 113 l methylcyclohexane
17. customdried at 50° C.