تفاعل #311399

معادلة التفاعل

lithium aluminum hydride

lithium aluminum hydride

methyl-α-[4-(4-trifluoromethylphenoxy)-phenoxy]propionate

sulfuric acid

→

desired product

المردود 79.3%

β-[4-(4-Trifluoromethylphenoxy)phenoxy]propanol

المردود 79.3%

المذيبات

diethyl ether

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwhile cooling
2. 2
   workup.ADDITIONAfter completion of the addition
3. 3
   أخرىthe reaction
4. 4
   workup.ADDITIONwas added to the mixture
5. 5
   أخرىThe ethereal layer was separated
6. 6
   استخلاصextracted twice with diethyl ether
7. 7
   تجفيفdried over anhydrous sodium sulfate
8. 8
   أخرىThe ether was removed from the dried
9. 9
   استخلاصextract
10. 10
    workup.DISTILLATIONthe resulting residue was distilled under reduced pressure

الإجراء التجريبي

6.6 g of methyl-α-[4-(4-trifluoromethylphenoxy)-phenoxy]propionate was dissolved in 15 ml of anhydrous diethyl ether, and the solution was added slowly to a dispersion of 0.4 g of lithium aluminum hydride in 50 ml of anhydrous diethyl ether while cooling. After completion of the addition, the mixture was refluxed at about 35° C. for 10 minutes to complete the reaction. The reaction mixture was poured into an appropriate amount of ice water to decompose any remaining unreacted lithium aluminum hydride, and 10% sulfuric acid was added to the mixture. The ethereal layer was separated, extracted twice with diethyl ether and dried over anhydrous sodium sulfate. The ether was removed from the dried extract and the resulting residue was distilled under reduced pressure to obtain 4.8 g of the desired product having a boiling point of 165° to 168° C./3 mmHg.

المصدر