tert-Butanol → HCID 13580615, compound

Participants

Reaction Steps

A mixture of 3-t-butoxycarbonylaminothiophene-2-carboxylic acid (10.0 g, 41.1 mmol), diphenylphosphoryl azide (14.14 g, 51.37 mmol) and triethylamine (5.85 ml, 42.2 mmol) in t-butyl alcohol (1000 ml) was stirred under reflux for 10 hours. The mixture was evaporated and the residue was dissolved in methylene chloride (300 ml). The solution was washed successively with 5% aqueous citric acid, water, saturated aqueous NAHCO3, followed by evaporation to give 5.9 g of a substance which was purified by recrystallization from heptane-methylene chloride to afford di-t-butyl thiophene-2,3-dicarbamate. M.p. 168°-170° C. Litt. m.p.: 165°-167° C. (J. Chem. Res. (S), 296, 1985).

Provenance & Evidence