3-Pyridinecarbonyl chloride, hydrochloride (1:1) → HCID 15157376, compound

Participants

Reaction Steps

To 1.5 ml of pyridine were added 1.0 g of 7-(1-methyl-2-propenyl)-8-hydroxy-5-methyl-9-methylamino-1,2,3,4,4a,9a-hexahydrofluorene and 0.7 g of nicotinoylchloride hydrochloride, followed by stirring at room temperature for 5 hours. The reaction mixture was concentrated and then extracted with chloroform. The chloroform layer was washed with water, dried with sodium sulfate and then concentrated. The residue was purified by a silica gel column chromatography (eluent: ethyl acetate) and then recrystallized from ethyl acetate-n-hexane to obtain 0.7 g of 7-(1-methyl-2-propenyl)-8-hydroxy-5-methyl-9-(N-methyl-N-nicotinoylamino)- 1,2,3,4,4a,9a-hexahydrofluorene having a melting point of 183°-184° C. and of colorless powdery crystal.

Provenance & Evidence