تفاعل #1583878

معادلة التفاعل

methanol

diisobutylaluminum hydride

methyl 2,2-diphenylacetate

sodium hydroxide

→

2,2-diphenyl ethanol

المردود 92.4%

المذيبات

dichloromethane

toluene

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the completion of dropwise addition
2. 2
   أخرىAfter the completion of reaction
3. 3
   أخرىat −20° C
4. 4
   أخرىAfter the completion of reaction
5. 5
   استخلاصfor extraction
6. 6
   غسيلThe organic phase was washed with water
7. 7
   تجفيفdried over anhydrous sodium sulfate
8. 8
   أخرىevaporated
9. 9
   أخرىto remove the solvent

الإجراء التجريبي

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%.

المصدر