تفاعل #1583873

معادلة التفاعل

ethyl 3,3-diphenyl-1-propanate

diisobutylaluminum hydride

methanol

water

→

3,3-diphenyl-1-propanol

المردود 100.2%

المذيبات

dichloromethane

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىTo a 30 L reaction kettle
2. 2
   workup.ADDITIONAfter the completion of dropwise addition
3. 3
   أخرىAfter the completion of reaction
4. 4
   أخرىto quench off
5. 5
   أخرىthe reaction
6. 6
   استخلاصextracted with dichloromethane
7. 7
   تجفيفThe organic phase was dried over anhydrous sodium sulfate
8. 8
   أخرىevaporated
9. 9
   أخرىto remove the solvent

الإجراء التجريبي

To a 30 L reaction kettle was slowly added a solution of diisobutylaluminum hydride in toluene (15 L, 1 mol/L) at −20° C. After stirring, to the resulting mixture was slowly added a solution of ethyl 3,3-diphenyl-1-propanate (1200 g, 4.7 mol) in dichloromethane dropwisely. After the completion of dropwise addition, the reaction was conducted at 25° C. for 12 hours. After the completion of reaction monitored by TLC, the reaction solution was divided into three parts. 200 mL methanol and 1000 mL water were slowly added respectively at −20° C. to quench off the reaction. The reaction solutions were combined and extracted with dichloromethane. The organic phase was dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce an oily crude product of 3,3-diphenyl-1-propanol (1000 g), which was directly used in the next reaction.

المصدر