HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-[6-Fluoro-3-(2-fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5-nitropyrimidine-4,6-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 59177864 | HCID 59177864 | — |
| Reactant | 6-Fluoro-3-(2-fluorobenzyl)-1H-pyrazolo[4,3-b]pyridine | HCID 178505974 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-[6-Fluoro-3-(2-fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5-nitropyrimidine-4,6-diamine | HCID 67516966 | — |
Reaction Steps
156 mg (about 66% pure, 0.636 mmol) of the compound from example 6A were dissolved in DMF (3.5 ml), 28 mg (0.70 mmol) of sodium hydride (60% in mineral oil) were then added and the mixture was stirred at RT for 2 h. 115 mg (0.604 mmol) of 2-chloro-5-nitropyrimidine-4,6-diamine (synthesis: Helvetica Chimica Acta (1951), 34, 835-40) were then added, and the reaction mixture was stirred at 80° C. for another 1 h. After cooling to RT, the mixture was added to water. The suspension obtained in this manner was filtered off and the solid was washed repeatedly with water and then dried under high vacuum. This gave 196 mg (77% of theory) of the title compound in solid form.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09090609B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-c92779079e9a4b4d81e7db4039c3d97e |
| Source note | uspto-grants-2015_07 |