Hydrogen iodide → HCID 178508570, compound

6-Chloro-9H-purin-2-amine (5.0 g., 29.5 mmole) was added to 47% hydrogen iodide (61 ml., 12.2 ml./g.) chilled in an ice bath. After 1.5 hours, water (61 ml.) was added and the mixture stirred in an ice-bath for 30 minutes. The yellow solid was filtered out and the filter cake was washed with water. The wet solid was transferred to a beaker and the residue in the funnel was washed into the beaker with water (30 ml.). 6M Sodium hydroxide (7 ml.) was added with stirring until all the solid had dissolved (pH 14). The solution was added to boiling water (30 ml.) containing acetic acid (3 ml.). The mixture was boiled briefly and allowed to stand at room temperature for one hour. The product was filtered off, washed with water, and dried under vacuum overnight to give 6.88 g. of the desired product; m.p. about 240° C. (dec.).

1. temperaturechilled in an ice bath
2. filtrationThe yellow solid was filtered out
3. washthe filter cake was washed with water
4. washthe residue in the funnel was washed into the beaker with water (30 ml.)
5. addition6M Sodium hydroxide (7 ml.) was added
6. stirringwith stirring until all the solid
7. dissolutionhad dissolved (pH 14)
8. additionThe solution was added
9. additioncontaining acetic acid (3 ml.)
10. waitto stand at room temperature for one hour
11. filtrationThe product was filtered off
12. washwashed with water
13. customdried under vacuum overnight
14. customto give 6.88 g

ORD record

ord-444c172a092b49c1af18a9619ca6a8ae

Source dataset

uspto-grants-1997_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05608064