反応 #985247

反応方程式

1-methylimidazole

chlorodiphenylphosphine

ethanol

→

ethoxydiphenylphosphine

収率 96.7%

反応条件

後処理

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
   その他The reactor was fitted with an overflow through which the reaction mixture
4. 4
   その他was held at 80° C
5. 5
   その他for the first 4 hours
6. 6
   その他The output over a duration of 1 hour was then collected
7. 7
   その他497.2 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
    その他gave 438.2 g of 99.74% EODPP

実験手順

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%.

出典