Hydrogen Bromide → HCID 178516000, compound

Participants

Reaction Steps

A mixture of XIX (2.9 g, 0.01 mole), glacial HOAc (10 mL) and 48% HBr (35 mL) was stirred at reflux for 3 hours. The hot solution was decanted from the separated tar and chilled at 5°-10° C. overnight. The precipitated hydrobromide salt was collected, washed with Et2O, dissolved in H2O (100 mL), and the solution was made basic with saturated NaHCO3 solution. The solid was collected, chromatographed on silica gel, and the product eluted with 95CHCl3 --5CH3OH--0.5H2O to yield 0.725 g (27%) of XX; m.p. 165.5°-167° C. (50% CH3OH).

Provenance & Evidence