Triethylamine → HCID 54242229, Verbindung

Temperatur

-15 °C

20.7 mg of L-N-[(2R or S)-5-ethylthio-2-(naphthylmethyl)pentanoyl]norleucine was dissolved in 0.5 ml of dry DMF. Then, 27.4 μl of triethylamine, 12.9 μl of DPPA and 20 mg of (2RS,4S,5S)-5-amino-2-ethyl-4-hydroxy-7-methyloctanoic acid isobutylamide monohydrochloride was added thereto under stirring at -15° C. The mixture was stirred at the same temperature for one hour and then at 5° C. overnight. The reaction solution was diluted with 20 ml of ethyl acetate, washed with water and with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=50/1) to obtain 16.9 mg of (2RS,4S,5S)-5-{L-N-[(2R or S)-5-ethylthio-2-(1-naphthylmethyl)pentanoyl]norleucyl}amino-2-ethyl-4-hydroxy-7-methyloctanoic acid isobutylamide as colorless solid.

1. stirringThe mixture was stirred at the same temperature for one hour
2. customat 5° C.
3. customovernight
4. washwashed with water and with a saturated sodium chloride aqueous solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThen, the solvent was distilled off under reduced pressure
7. customThe residue was purified by silica gel column chromatography (chloroform/methanol=50/1)

ORD-Eintrag

ord-b6084522f7014ffaa529682d1bee6a84

Quelldatensatz

uspto-grants-1996_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05481036