Dichlorodimethylsilane → 2,6-Dichloropurine

Temperature

55 °C

2-Amino-6-chloropurine (5.00 g, 29.5 mmol), dichlorodimethylsilane (11.42 g, 88.5 mmol), benzyltriethylammonium chloride (0.40 g, 1.8 mmol) and isoamyl nitrite (5.18 g, 44.2 mmol) were added to heptane (25 ml), and the mixture was heated to 50-60° C. and stirred for 17 hr. After the completion of the reaction, the mixture was filtrated. The obtained crystals were diluted with water (25 ml) and 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 recrystallized from methanol. The mixture was dried under reduced pressure at 60° C. to give 2,6-dichloropurine as a white powder (3.68 g, yield 66.1%). 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 (25 ml)
4. temperaturecooling for 1 hr
5. filtrationthe mixture was filtrated
6. customthe obtained crystals were recrystallized from methanol
7. customThe mixture was dried under reduced pressure at 60° C.

ORD record

ord-12f7874803fb45e8ba94689986d0eddc

Source dataset

uspto-grants-2007_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07307167B2