Cyanogen Bromide → HCID 22816303, compound

Participants

Reaction Steps

To a suspension of Compound 7A (9.39 g, 30 mmole; prepared in Example 7A) and powdered anhydrous K2CO3 (6.00 g, 47 mmole) in 60 ml of chloroform was added a solution of cyanogen bromide in chloroform (1.2 eq, 1.0 g/20 ml) dropwise. Stirring was continued for 30 min at about 20° C. after which the mixture was refluxed for 2 hr. After cooling the mixture, the insoluble material therein was removed by filtration. The filtrate was evaporated to a syrup which crystallized upon azeotropic distillation with ethanol. The crystals were boiled with 40 ml of ethanol and collected after storage at 5° C. overnight to give 7.93 g (82% yield) of product, mp 237°-241°.

Provenance & Evidence