Fmoc-Gly-OH → HCID 22877916, Verbindung

Temperatur

60 °C

Two grams (6.3 mmols) of (Z)-1-(3-amino-4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-ethene, 2.3 g of Fmoc-Gly and 11 g (25 mmols) of a BOP reagent were dissolved in 40 ml of N,N-dimethylformamide, and the mixture was heated at 60° C. for 2 hours. After the reaction mixture was cooled, a saturated aqueous solution of sodium hydrogencarbonate was added thereto. The resulting mixture was extracted three times with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure. The product was purified through silica-gel column chromatography (mixture of ethyl acetate and hexane at a ratio by volume of 1:2) to give 1.63 of the final product in a yield of 43.5%.

1. temperatureAfter the reaction mixture was cooled
2. extractionThe resulting mixture was extracted three times with dichloromethane
3. dry with materialThe extract was dried over anhydrous sodium sulfate
4. concentrationconcentrated to dryness under reduced pressure
5. customThe product was purified through silica-gel column chromatography (
6. additionmixture of ethyl acetate and hexane at a ratio by volume of 1:2)

ORD-Eintrag

ord-272e797406da49cd9d4a1eafd9e6f103

Quelldatensatz

uspto-grants-1997_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05674906