تفاعل #90036

معادلة التفاعل

4-(3-Cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester

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title compound

4-(3-Cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl)-piperidine-1-carboxylic acid tert-butyl ester

المذيبات

THF

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe solid was filtered through Celite
2. 2
   غسيلeluted with a mixture solvent (400 ml; THF/methanol=4/1)
3. 3
   تركيزconcentrated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residues were dissolved in ethyl acetate (400 ml)
5. 5
   غسيلwashed with 1% aqueous solution of N-acetylcysteine, saturated aqueous solution of NaHCO3 and saturated brine
6. 6
   تجفيفThe organic layer was dried over sodium sulfate
7. 7
   أخرىThe drying agent was removed by filtration
8. 8
   تركيزthe residues were concentrated under reduced pressure

الإجراء التجريبي

4-(3-Cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (Compound B2-22-1, 16.2 g, 34.6 mmol) was dissolved in THF (800 ml) and methanol (230 ml), added with 10 wt % Pd/C (3.2 g), and stirred under hydrogen atmosphere for 19 hr. The solid was filtered through Celite, eluted with a mixture solvent (400 ml; THF/methanol=4/1), and concentrated under reduced pressure. The residues were dissolved in ethyl acetate (400 ml), and then washed with 1% aqueous solution of N-acetylcysteine, saturated aqueous solution of NaHCO3 and saturated brine. The organic layer was dried over sodium sulfate. The drying agent was removed by filtration and the residues were concentrated under reduced pressure to obtain the title compound as a crude product (white powder, 14.0 g, 86%).

المصدر