反応 #1583873

反応方程式

ethyl 3,3-diphenyl-1-propanate

diisobutylaluminum hydride

methanol

water

→

3,3-diphenyl-1-propanol

収率 100.2%

溶媒

dichloromethane

toluene

反応条件

後処理

1. 1
   その他To a 30 L reaction kettle
2. 2
   workup.ADDITIONAfter the completion of dropwise addition
3. 3
   その他After the completion of reaction
4. 4
   その他to quench off
5. 5
   その他the reaction
6. 6
   抽出extracted with dichloromethane
7. 7
   乾燥The organic phase was dried over anhydrous sodium sulfate
8. 8
   その他evaporated
9. 9
   その他to remove the solvent

実験手順

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.

出典