HCID 178453385, compound → beta-Amanitin hexamethylenediamide

Participants

Reaction Steps

4.54 mg (4.05 μmol) β-Amanitin-(t-butyloxy-carbonyl)-hexamethylenediamide (I) was stirred at room temperature in 250 μl trifluoroacetic acid. After 2 minutes the excess TFA was evaporated at 20° C. and the remaining solid coevaporated 2 times with 1 ml acetonitrile and methanol. The crude amine was dissolved in 1000 μl dmso and prified on a LaPrep-HPLC: column: Kromasil 100-C18, 10 μm, 250×20 mm, with methanol/water (0.05% TFA), flow: 26 ml/min, detection at λ295 nm. Solvent A: 95% water: 5% methanol 0.05% trifluoroacetic acid. Solvent B: 10% water: 90% methanol 0.05% trifluoroacetic acid. Gradient: 0-5 min 100% A; 5-20 25 min 0% A; 25-27 min 100% A; 27-35 min 100% A. The fractions with the same retention time were collected and the solvents evaporated.

Provenance & Evidence