Triphenylphosphine → HCID 69999615, compound

Participants

Reaction Conditions

Reaction Steps

500 mg polymerbound triphenylphosphine (Fluka #93093) was added to 267 mg (0.55 mmol) 6-{(5-acetylamino-2-azido-benzoyl)-cyclohexylcarbamoylmethyl-amino}-hexanoic acid methyl ester in 8 ml 1,2-dichloroethane. The suspension was heated to 50° C. for 120 min and the solvent was filtered off. The solid was collected, suspended in a solution consisting of 8 ml AcOH, 1 ml water, and 1 ml dioxane and the mixture was heated to reflux for 24 h and filtered. The filtrate was concentrated in vacuo and the residue flashchromatographed on silicagel in EtOAc/hexane as eluent to yield 6-(7-acetylamino-2,5-dioxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepin-4-yl)-hexanoic acid methyl ester (117 mg, 0.32 mmol): MS (ISP) 362(M+H)+.

Provenance & Evidence