HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 11464606, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | 6-Methoxycarbonyl-2-{2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidin-1-yl}-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidine | HCID 11305382 | — |
| Product | HCID 11464606 | HCID 11464606 | 93% |
Reaction Steps
A mixture of 6-methoxycarbonyl-2-{2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidin-1-yl}-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidine (Example 56) (200 mg, 0.45 mmol) and a solution of 7N ammonia in methanol (7 ml, 49 mmol) was heated at 65° C. in a sealed vessel under microwave irradiation for 1 hour. The reaction mixture was evaporated, dissolved in methanol and passed through a 50 g isolute SCX-2 ion exchange column. The column was eluted with methanol to elute any neutrals, followed by 7M methanolic ammonia to elute the product. The solvent was removed by evaporation and the residue triturated with diethylether. The resulting solid was collected by filtration to give the title compound (180.0 mg, 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07579349B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-0566f0426aad45928672ea7be60a9d89 |
| Source note | uspto-grants-2009_08 |