反応 #90067

反応方程式

(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

収率 66.0%

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

収率 66.0%

溶媒

methanol

THF

反応条件

後処理

1. 1
   抽出was then extracted with ethyl acetate
2. 2
   洗浄The organic layer was washed with brine
3. 3
   乾燥dried over magnesium sulfate
4. 4
   その他The solids obtained
5. 5
   ろ過after filtration and concentration under reduced pressure
6. 6
   洗浄were washed with dichloromethane
7. 7
   その他purified by HPLC

実験手順

(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%).

出典