反応 #1583878

反応方程式

methanol

diisobutylaluminum hydride

methyl 2,2-diphenylacetate

sodium hydroxide

→

2,2-diphenyl ethanol

収率 92.4%

溶媒

dichloromethane

toluene

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONAfter the completion of dropwise addition
2. 2
   その他After the completion of reaction
3. 3
   その他at −20° C
4. 4
   その他After the completion of reaction
5. 5
   抽出for extraction
6. 6
   洗浄The organic phase was washed with water
7. 7
   乾燥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 500 mL three-opening flask was slowly added a solution of diisobutylaluminum hydride in toluene (282 mL, 1 mol/L) at −30° C. After stirring, to the resulting mixture was slowly added a solution of methyl 2,2-diphenylacetate (21 g, 92.8 mmol) 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, to the resulting mixture was slowly added methanol (10 mL), dichloromethane (100 mL) and an aqueous sodium hydroxide solution (100 mL, 1 mol/L) at −20° C. After the completion of reaction, to the reaction solution was added dichloromethane for extraction. The organic phase was washed with water, dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce 2,2-diphenyl ethanol (17 g) in a yield of 92.4%.

出典