Diethylamine → HCID 58078467, compound

Participants

Reaction Steps

A 500-mL round-bottom flask was charged with Fmoc-L-phenylalanine-2,4-dimethoxybenzyl ester (26.00 g, 48.3 mmol), CH2Cl2 (150 mL) and diethylamine (75 mL, Acros). Mixture was stirred at room temperature and the completion monitored by HPLC. After 4 h, the mixture was concentrated (bath temp<30° C.). The residue was resuspended in CH2Cl2 (200 mL) and concentrated. This was repeated once. To the residue was added MeOH (20 mL), which caused the formation of a gel. This residue was diluted with CH2Cl2 (200 mL), concentrated and the cloudy oil left under vacuum overnight. The residue was suspended in CH2Cl2 (100 mL), then toluene (120 mL) was added. The mixture was concentrated and the residue left under vacuum overnight.

Provenance & Evidence