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. Methylpiperazine (9.0 g) and triethylamine (8 ml) are added to the bottle. The above mixture is reacted at 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 amount of solid is separated out. After filtration, a filter cake is washed with ethyl acetate for 3 times and then dried in vacuum for 5 h at to obtain solid purin (12.0 g). The yield is about 67.4%.

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

ORD record

ord-cc3927e6c9fc46fbbdf11776f26cab34

Source dataset

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08580763B2