Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Glycine | HCID 750 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | N-(3-chlorophenyl)-4-(2-chloropyridin-4-yl)pyrimidin-2-amine | HCID 9905031 | — |
| Solvent | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Product | HCID 21948244 | HCID 21948244 | — |
Reaction Steps
A mixture of (3-chloro-phenyl)-[4-(2-chloro-pyridin-4-yl)-pyrimidin-2-yl]-amine (10.0 g, 0.03 mol) and glycine (4.8 g, 0.06 ml) in DBU (100 ml) is heated at 150° C. under an atmosphere of argon for 40 hours. The still hot reaction mixture is poured into water. After washing the aqueous phase with ethyl acetate the pH is adjusted to 5 by adding citric acid. The resulting precipiate is filtered and recrystallized from dimethylformamide/ethanol to give the product in form of yellow crystals, m.p. 136–138° C. (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07109197B2 |
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| Source dataset | uspto-grants-2006_09 |
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| ORD ID | ord-a9c540219bf6449e8e03def5bc7bb29b |
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| Source note | uspto-grants-2006_09 |
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