Water → HCID 22007318, Verbindung

1.3 g (9.44 mmol) of potassium carbonate were added at 60° C. to a solution of 2.4 g (5.9 mmol) of 3-methyl-7-tritylxanthine from stage a) in 50 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 1.06 ml (7.67 mmol) of benzyloxymethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 7 hours. 50 ml of water were then added and the mixture was extracted three times using 60 ml of methyl tert-butyl ether each time. The combined organic phases were washed twice with 30 ml of water each time, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2).

1. stirringthe mixture was stirred at 80° C. for 7 hours
2. extractionthe mixture was extracted three times
3. washThe combined organic phases were washed twice with 30 ml of water each time
4. customdried
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2)

ORD-Eintrag

ord-43c493a903f4471eb3efe46a36545df3

Quelldatensatz

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06214992B1