3,4-dihydro-2H-pyran → Purine

In a 100 ml three-mouth bottle, 2,6-dichloropurine (10 g), ethyl acetate (50 ml), pyridinium salt of paratoluenesulfonic acid (0.2 g) are mixed. The above mixture is stirred and heated to a temperature of 35° C., 2,3-dihydropyrane (12 ml) is added thereto within 5 min. The above mixture is reacted at 50˜60° C. for 3 h. The completion of reaction is checked with TCL analysis. Triethylamine (7.9 ml) is added to the bottle, and DL-aminopropanol (7.0 ml) is added thereto under the temperature. The above mixture is reacted under the temperature for 1 h. The completion of reaction is checked with TCL analysis. The reaction mixture is cooled to room temperature. After filtration, a filter cake is completely washed with ethyl acetate, and a filtrate is washed with water for 3 times and delaminated. Organic layer is concentrated till large amounts of solid is separated out. After filtration, a filter cake is washed with ethyl acetate for 3 times and then dried in vacuum at 50° C. for 5 h to obtain solid purin (11.6 g). The yield is about 70.4%.

1. additionis added
2. customThe above mixture is reacted at 50˜60° C. for 3 h
3. customThe completion of reaction
4. additionis added
5. customThe above mixture is reacted under the temperature for 1 h
6. customThe completion of reaction
7. filtrationAfter filtration
8. washa filter cake is completely washed with ethyl acetate
9. washa filtrate is washed with water for 3 times
10. concentrationOrganic layer is concentrated till large amounts of solid
11. customis separated out
12. filtrationAfter filtration
13. washa filter cake is washed with ethyl acetate for 3 times
14. customdried in vacuum at 50° C. for 5 h

ORD record

ord-2664148dd03c4182a0f45ebb84d85c06

Source dataset

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08580763B2