Citric Acid → HCID 131713638, compound

Participants

Reaction Steps

A mixture of 9.25 g. (0.025 mole) of (+)-ethyl-1-(2'-methoxycarbonyl-2'-hydroxyimino-ethyl)-1,2,3,4,6,7,12,12b-octahydro-indolo[2,3-a]quinolizine, 8.0 g (0.2 mole) of solid sodium hydroxide, 100 ml. of ethanol and 5.0 ml. of water is acidified to a pH value of 6.3 by the addition of a solution of 16 g. of citric acid in 150 ml. of water. The solution is extracted six times with 50 ml. of dichloromethane each. The united organic phases are extracted with a saturated sodium chloride solution, the layers are separated, the organic phase is dried over anhydrous sodium sulfate, filtered and the filtrate is evaporated. To the residue 50 ml. of ether are added, the mixture is heated to boiling, then cooled, the precipitated product is filtered and dried. Thus 7.2 g. of the named compound are obtained, yield 81%. Mp.: 124° C. (decomposition).

Provenance & Evidence