Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Allyl Alcohol | HCID 7858 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Amino-4,6-difluoropyrimidine | HCID 1201480 | — |
| Product | HCID 14717228 | HCID 14717228 | — |
Reaction Steps
1.14 g (0.0382 mol) of 80% sodium hydride (emulsion in linseed oil) were added at 25° C. under a nitrogen atmosphere to 70 ml of allyl alcohol. To the clear solution obtained after stirring at 40° C. for 20 minutes were added 5.0 g (0.0382 mol) of 2-amino-4,6-difluoropyrimidine, and the mixture was then stirred at 97° C. for 1.5 hours. To work up, the excess alcohol was removed by distillation under reduced pressure, the residue was taken up in methylene chloride, and the solution was washed with water, dried over magnesium sulfate and then freed of solvent. The viscous oil obtained in this way crystallized on trituration with n-pentane. 4.6 g (71.2% of theory) of the title compound of melting point 62°-66° C. were obtained after filtering off, washing with water and drying.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05011927 |
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| Source dataset | uspto-grants-1991_04 |
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| ORD ID | ord-cdb743a18ba54b09a13a36eff7018a6c |
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| Source note | uspto-grants-1991_04 |
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