Acetic Acid → HCID 131718931, compound

Participants

Reaction Steps

The Z-Leu-Leu-CH2F (0.39 g) obtained in Example 3 was dissolved in acetic acid (5 ml) including a 25% anhydrous hydrogen bromide and the mixture was agitated at room temperature for 3 hours. After the end of the reaction, the solvent was distilled off and the resultant residue was dissolved in anhydrous methylene chloride (5 ml). To this, under ice water, were added triethylamine (0.23 g) and octanoylchloride (0.2 g) to dissolve it, then this was washed with a 10% aqueous citric acid solution, a 5% sodium hydrogencarbonate, then a saturated saline water in this order, then was dried on anhydrous sodium sulfate and the solvent distilled off under reduced pressure. The residue was purified by silica gel medium pressure column chromatography to obtain the above-referenced compound Octanoyl-Leu-Leu-CH2F (200 mg, 0.52 mmole) at a yield of 52%.

Provenance & Evidence