تفاعل #1131658

معادلة التفاعل

ammonia

3-hydroxy-2-methyl-3-phenyl-1-(8-quinolyl)cyclopentene

water

hydrochloric acid

→

2-methyl-3-phenyl-1-(8-quinolyl)cyclopentadiene

المردود 69.3%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىThe aqueous phase was then separated off from the organic phase
2. 2
   استخلاصthe aqueous phase was extracted twice with diethyl ether
3. 3
   تجفيفdried over magnesium sulfate
4. 4
   ترشيحfiltered
5. 5
   workup.DISTILLATIONthe solvent was distilled off
6. 6
   أخرىThe residue obtained in this way
7. 7
   workup.DISTILLATIONwas distilled at 157-170° C.

الإجراء التجريبي

A mixture of 5 ml of water and 5 ml of concentrated hydrochloric acid was added to a solution of 1.717 g (5.7 mmol) of 3-hydroxy-2-methyl-3-phenyl-1-(8-quinolyl)cyclopentene in 100 ml of tetrahydrofuran. The mixture was stirred at room temperature for 90 minutes and ammonia solution was then added until the pH was 12. The aqueous phase was then separated off from the organic phase and the aqueous phase was extracted twice with diethyl ether. The organic phases were combined, dried over magnesium sulfate, filtered and the solvent was distilled off. The residue obtained in this way was distilled at 157-170° C. and 2×10−2 mbar to give 1.12 g (3.95 mmol, 69.3%) of 2-methyl-3-phenyl-1-(8-quinolyl)cyclopentadiene.

المصدر