Sodium Bicarbonate → HCID 54011493, compound

Participants

Reaction Steps

A mixture of 3,5-bis(acetylamino)-2,4,6-triiodobenzoyl chloride (32 g, 50 mmol), N-(2,3-dihydroxypropyl)-3-aminomethyl-2,2,5,5-tetramethyl-1-pyrrolidinyloxy, free radical (12.3 g, 50 mmol) and sodium bicarbonate (4.2 g, 50 mmol) in 100 mL of dimethyl formamide is stirred for 18 hours at room temperature. The solvent is evaporated under reduced pressure. The residue is purified by C18 chromatography to give the spin labelled triiodobenzenecarboxamide. The chemical reaction is shown below: ##STR24## A mixture of N-((2,2,5,5-tetramethyl-1-pyrrolidinyloxy)methyl, free radical)-N-(2,3-dihydroxypropyl)-3,5-bis(acetylamino)-2,4,6-triiodobenzenecarboxamide (21 g, 25 mmol), sodium trifluoroacetate (61.2 g, 450 mmol) and copper(I) iodide (42.8 g, 225 mmol) in 500 mL of N,N dimethylacetamide is refluxed under argon for six hours. The solvent is evaporated under reduced pressure. The residue is purified by C18 chromatography to give N-((2,2,5,5-tetramethyl-1-pyrrolidinyloxy)methyl, free radical)-N-(2,3-dihydroxypropyl)-3,5-bis(acetylamino)-2,4,6-tris(trifluoromethyl)benzenecarboxamide. The chemical reaction is shown below: ##STR25##

Provenance & Evidence