Hydrochloric Acid → HCID 54549745, compound

Participants

Reaction Conditions

Reaction Steps

9.02 g (13.8 mmol) of 3i are dissolved in 140 ml of tetrahydrofuran. After addition of 100 ml of 2M hydrochloric acid the mixture is heated at 50° C. for 4 hours. The mixture becomes turbid and on cooling a colorless precipitate separates, which is filtered off and first washed with a little THF and then with water. The solid is dried in a vacuum desiccator. 4.50 g of colorless powder of m.p. 137° C. are obtained. The mother liquor is concentrated, extracted a number of times with dichloromethane, the extracts are dried with magnesium sulfate, the solvent distilled off and the resulting oily residue is chromatographed with isohexane/acetic ester mixtures on a silica gel column. A total of 5.90 g (75%) of product are isolated.

Provenance & Evidence