Chlorotrimethylsilane → 2,6-Dichloropurine

Temperatur

55 °C

9-Acetyl-2-amino-6-chloropurine (0.50 g, 2.36 mmol), tetraethylammonium chloride (0.025 g, 0.15 mmol) and isoamyl nitrite (0.42 g, 3.54 mmol) were added to chlorotrimethylsilane (4.0 g, 36.8 mmol), and the mixture was heated to 50-60° C. and stirred for 10 hr. After the completion of the reaction, the mixture was filtrated. The obtained crystals were diluted with water (4.0 ml), and the mixture was adjusted to pH 4-5 with a 2M aqueous sodium hydroxide solution. After aging under ice-cooling for 1 hr, the mixture was filtrated, and the obtained crystals were dried under reduced pressure at 80° C. to give 2,6-dichloropurine as a white powder (0.35 g, yield 78.3%). The properties of the obtained compound were the same as in Example 1(2).

1. customAfter the completion of the reaction
2. filtrationthe mixture was filtrated
3. additionThe obtained crystals were diluted with water (4.0 ml)
4. temperaturecooling for 1 hr
5. filtrationthe mixture was filtrated
6. customthe obtained crystals were dried under reduced pressure at 80° C.

ORD-Eintrag

ord-bb49f1bde22b487c8c4ff306dbe3e3d5

Quelldatensatz

uspto-grants-2007_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07307167B2