Reaktion #1134641

Reaktionsgleichung

hydrochloric acid

( VI )

4-(2-amino-6-chloro-4,5-dihydropurin-9-yl)-3-methylene-2-trityloxymethyl-cyclopentanol

sodium hydroxide

→

title compound

Ausbeute 73.1%

2-amino-9-(4-hydroxy-3-hydroxymethyl-2-methylene-cyclopentyl)-1,9-dihydropurin-6-one

Ausbeute 73.1%

Lösungsmittel

Acetonitril

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith heating
2. 2
   SonstigeAfter completion of the reaction
3. 3
   Temperaturthe resulting mixture was cooled to room temperature
4. 4
   Waschenwashed with ethyl acetate
5. 5
   Sonstigeto remove tritylcarbinol
6. 6
   SonstigeThe material thus obtained
7. 7
   workup.STIRRINGstirred at 90° C. for 1 hr
8. 8
   SonstigeThe solution thus obtained
9. 9
   workup.STIRRINGwas stirred
10. 10
    Temperaturwith cooling slowly to room temperature
11. 11
    workup.STIRRINGfurther stirred at room temperature for 1 hr
12. 12
    Sonstigeto obtain crystal
13. 13
    TemperaturThe resulting material was cooled to 6° C.
14. 14
    workup.STIRRINGstirred for 1 hr

Vorschrift

Acetonitril (30 ml) and 2N aqueous hydrochloric acid (23.3 ml) were added to the compound of formula (VI) obtained in Example 1-8 (1.38 g, 2.56 mmol) and stirred at 82° C. for 12 hrs with heating. After completion of the reaction, the resulting mixture was cooled to room temperature and washed with ethyl acetate to remove tritylcarbinol. The material thus obtained was neutralized to pH 6.8 by using 3N aqueous sodium hydroxide (13.6 ml) and stirred at 90° C. for 1 hr. The solution thus obtained was stirred with cooling slowly to room temperature and further stirred at room temperature for 1 hr to obtain crystal. The resulting material was cooled to 6° C. and stirred for 1 hr to obtain the title compound (0.554 g, yield: 73.1%).

Quelle