تفاعل #1184562

معادلة التفاعل

ethyl 4-[N-ethyl-(5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)amino]benzoate

sodium hydroxide

hydrochloric acid

→

title compound

المردود 79.0%

4-[N-Ethyl-(5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)amino]benzoic acid

المردود 79.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.WAITThe reaction mixture was left
2. 2
   درجة الحرارةto cool
3. 3
   استخلاصthe mixture was extracted with chloroform
4. 4
   غسيلThe organic layer was washed with saturated brine
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   تركيزThe organic layer was concentrated under reduced pressure
7. 7
   أخرىthe resulting residue was recrystallized from ethanol

الإجراء التجريبي

A suspension of ethyl 4-[N-ethyl-(5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)amino]benzoate (0.036 g) in ethanol (5 ml) was added with 20% aqueous sodium hydroxide (1 ml), and the mixture was stirred overnight at 50° C. The reaction mixture was left to cool and then made acidic with 2 N aqueous hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from ethanol to obtain the title compound (0.026 g, yield: 79%) as colorless needles (melting point: 284-285° C.).

المصدر