Dichlorodimethylsilane → 2,6-Dichloropurine

Temperature

27.5 °C

9-Acetyl-2-amino-6-chloropurine (2.50 g, 11.8 mmol), dichlorodimethylsilane (4.57 g, 35.4 mmol), benzyltriethylammonium chloride (0.16 g, 0.70 mmol) and isoamyl nitrite (2.07 g, 17.7 mmol) were added to o-dichlorobenzene (10 ml), and the mixture was heated to 25-30° C. and stirred for 8 hr. After the completion of the reaction, the mixture was filtrated. The obtained crystals were diluted with water (4.0 ml), and the reaction mixture was added dropwise to 2M aqueous sodium hydroxide solution (20 ml) and partitioned. The aqueous layer was adjusted to pH 4-5 with 35% hydrochloric acid. 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 (1.62 g, yield 72.6%). 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. additionthe reaction mixture was added dropwise to 2M aqueous sodium hydroxide solution (20 ml)
5. custompartitioned
6. temperaturecooling for 1 hr
7. filtrationthe mixture was filtrated
8. customthe obtained crystals were dried under reduced pressure at 80° C.

ORD record

ord-575825576c19492d8de4acc092c51aeb

Source dataset

uspto-grants-2007_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07307167B2