تفاعل #90067

معادلة التفاعل

(3-Cyano-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl)-propynoic acid methyl ester

Hydrochloric acid

→

title compound

المردود 66.0%

(3-Cyano-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl)-propynoic acid

المردود 66.0%

المذيبات

methanol

THF

ظروف التفاعل

المعالجة

1. 1
   استخلاصwas then extracted with ethyl acetate
2. 2
   غسيلThe organic layer was washed with brine
3. 3
   تجفيفdried over magnesium sulfate
4. 4
   أخرىThe solids obtained
5. 5
   ترشيحafter filtration and concentration under reduced pressure
6. 6
   غسيلwere washed with dichloromethane
7. 7
   أخرىpurified by HPLC

الإجراء التجريبي

(3-Cyano-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl)-propynoic acid methyl ester (Compound E6-1, 15.2 mg, 0.038 mmol) was dissolved in a mixture solvent of methanol (1.5 mL) and THF (0.5 mL), added with 2 N aqueous solution of potassium hydroxide (5 drops), and then stirred at room temperature overnight. 0.5 N Hydrochloric acid was added to the reaction solution, which was then extracted with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate. The solids obtained after filtration and concentration under reduced pressure were washed with dichloromethane and purified by HPLC to obtain the title compound (white solid, 9.6 mg, 66%).

المصدر