tert-Butanol → HCID 86665962, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 3,5-bis-(4-cyano-phenoxy)-benzoic acid (2.0 g, 5.6 mmol), diphenylphosphorylazide (1.2 ml, 5.6 mmol) and DIPEA (1 ml, 5.6 mmol) were dissolved in 20 ml of tert-butanol and stirred overnight at 80° C. Reaction mixture was cooled and diluted with 50 ml saturated solution of sodiumhydrogencarbonate and extracted with ethylacetate (3×50 ml). Combined organic layer was washed with 2×50 ml saturated solution of brineand dried over anhydrous sodium sulphate. Solvent was evaporated under vacuo and thus obtained crude product was subjected to column chromatography using silica gel as an absorbent and eluted with 10-20% mixture of ethylacetate and hexane to afford 1.0 g of the required product. Percentage purity (LCMS): 89.6%, (M+1)=427.1+1.

Provenance & Evidence