Water → HCID 22007304, 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 (prepared according to Example 17a) in 50 ml of N-methylpyrrolidone and the mixture was stirred at this temperature for one hour. 1.57 g (7.67 mmol) of 2-(4-chlorobenzyloxy)ethyl chloride were then added dropwise and the mixture was stirred at 80° C. for one hour. A further 1.0 g (4.9 mmol) of 2-(4-chlorobenzyloxy)ethyl chloride was then added and the mixture was stirred again for one hour. 50 ml of water were then added, the mixture was extracted three times using 60 ml of methyl tert-butyl ether each time, and 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 one hour
2. stirringthe mixture was stirred again for one hour
3. extractionthe mixture was extracted three times
4. washthe combined organic phases were washed twice with 30 ml of water each time
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2)

ORD-Eintrag

ord-12e1351a79ff47619b58315c6d38dbef

Quelldatensatz

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06214992B1