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Summary for Patent: 4,642,346
|Title:||Anhydrous crystalline 9-(1,3-dihydroxy-2-propoxymethyl)guanine|
|Abstract:||Novel anhydrous crystalline 9-(1,3-dihydroxy-2-propoxymethyl)guanine useful as an antiviral agent.|
|Inventor(s):||Chan; Tai W. (Palo Alto, CA), Nguyen; Huong T. (Saratoga, CA)|
|Assignee:||Syntex (U.S.A.) Inc. (Palo Alto, CA)|
1. Anhydrous crystalline 9-(1,3-dihydroxy-2-propoxymethyl)guanine.
2. The anhydrous crystals of claim 1 further characterized by water of hydration of less than 1% w/w.
3. The anhydrous crystals of claim 2 further characterized by m.p. 243.degree. C.-245.degree. C.
4. The anhydrous crystals of claim 3 characterized by the powder X-ray diffraction pattern shown in FIGS. IA, IB or IC.
5. The process for preparing the anhydrous crystals of claim 1 which comprises
(i) adding 9-(1,3-dihydroxy-2-propoxymethyl)guanine to a heated oxygen-containing solvent;
(ii) cooling the mixxture formed in step (i) to room temperature; and
(iii) recovering the crystals formed in step (ii).
6. The process of claim 5 wherein the oxygen-containing solvent is dimethyl acetamide or water.
7. The process of claim 6 wherein the solvent is warmed to 60.degree. to 100.degree. C.
8. The process of claim 7 which further comprises adding methanol or acetone to the warm solution.
9. The process of claim 5 wherein the oxygen-containing solvent is an alcohol of one to four carbon atoms.
10. The process of claim 9 wherein the solvent is warmed to 40.degree. to 80.degree. C.
11. A process for preparing the anhydrous crystals of claim 1 which comprises heating a suitable form of 9-(1,3-dihydroxy-2-propoxymethyl)guanine.
12. The process of claim 11 wherein the suitable form is 9-(1,3-dihydroxy-2-propoxymethyl)guanine hydrate.
13. The process of claim 12 wherein the hydrate is heated to 200.degree.-220.degree. C.
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