m-Chloroperbenzoic acid → HCID 131717972, compound

Participants

Reaction Steps

Dissolve 1,9-bis[4-methylmercaptophenyl]-1,5,9-triazanonane (1.88 g, 5 mmol) in chloroform (20 mL) and treat with metachloroperbenzoic acid (863 mg, 5 mmol). Add calcium hydroxide (556 mg, 7.5 mmol) and stir for 15 minutes. Filter and evaporate the solvent in vacuo. Dissolve the residue in trifluoroacetic anhydride (10 mL) and heat at reflux for 30 minutes. Evaporate the volatiles in vacuo and dissolve the residue in a mixture of methanol-triethylamine (1:1, 100 mL) and evaporate the solvent in vacuo. Dissolve the resdiue in chloroform, wash with saturated ammonium chloride and dry (MgSO4). Evaporate the solvent in vacuo to give the crude 1,9-bis[(4-mercaptophenyl)]-1,5,9 triazanonane.

Provenance & Evidence