반응 #985247

반응 방정식

1-methylimidazole

chlorodiphenylphosphine

ethanol

→

ethoxydiphenylphosphine

수율 96.7%

반응 조건

후처리

1. 1
   workup.ADDITIONA nitrogen-inertized reactor with a three-part pitched blade stirrer was continuously charged at 80° C. with the following feedstocks
2. 2
   workup.ADDITIONStream 1) was added at 330 ml/h and stream 2) at 380 ml/h
3. 3
   기타The reactor was fitted with an overflow through which the reaction mixture
4. 4
   기타was held at 80° C
5. 5
   기타for the first 4 hours
6. 6
   기타The output over a duration of 1 hour was then collected
7. 7
   기타497.2 g of upper phase and 280.8 g of lower phase were collected
8. 8
   workup.DISTILLATIONThe upper phase was then distilled under reduced pressure through a column
9. 9
   workup.ADDITIONfilled with Raschig rings, which
10. 10
    기타gave 438.2 g of 99.74% EODPP

실험 절차

A nitrogen-inertized reactor with a three-part pitched blade stirrer was continuously charged at 80° C. with the following feedstocks: 1) a mixture of 110.7 g of ethanol and 205.8 g of 1-methylimidazole 2) chlorodiphenylphosphine (99.4%). Stream 1) was added at 330 ml/h and stream 2) at 380 ml/h. Both feeds were below the surface. The reactor was fitted with an overflow through which the reaction mixture could continuously run out. The reactor volume below the overflow was 710 ml. The reaction temperature was held at 80° C. In order to bring the system to equilibrium, the output for the first 4 hours was discarded. The output over a duration of 1 hour was then collected and a mass balance conducted. The output consisted of two liquid phases. Over one hour, 497.2 g of upper phase and 280.8 g of lower phase were collected. 96.8% of the upper phase was EODPP. The upper phase was then distilled under reduced pressure through a column filled with Raschig rings, which gave 438.2 g of 99.74% EODPP. Together with the EODPP in the first fraction, the total yield was 96.7%.

출처