Triethylamine → HCID 57526554, compound

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Reaction Steps

To a mixture of the acid, 13-cyclohexyl-10-((((dimethylamino)sulfonyl)amino)carbonyl)-3-(methyloxy)-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-6-carboxylic acid, (427.2 mg, 0.79 mmol) in a mixture of PhMe/CH2Cl2 (6 ml/2 ml) at r.t. under N2 was added triethylamine (117 mg, 1.16 mmol), followed by diphenylphosphoryl azide (DPPA) (320 mg, 1.16 mmol). The mixture was stirred at r.t. for 4 hr. The volatiles were then evaporated. The residue was titurated with hydrochloric acid (3× 10 ml, 1N), dried and the crude azide, 13-cyclohexyl-10-((((dimethylamino)sulfonyl)amino)carbonyl)-3-(methyloxy)-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-6-carbonyl azide, was used without further purification Analytical HPLC method: Solvent A=10% MeOH-90% H2O-0.1% TFA, Solvent B=90% MeOH-10% H2O-0.1% TFA, Start % B=0, Final % B=100, Gradient time=2 min, Flow Rate=5 ml/min, Column: Xterra MS C18 S7 3.0×50 mm; LC/MS: (ES+) m/z (M+H)+=565.21, HPLC Rt=1.988 min.

Provenance & Evidence