HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 59639627, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| Reactant | HCID 66892925 | HCID 66892925 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59639627 | HCID 59639627 | — |
Reaction Steps
To a solution of the product of Example 230(a), 2-amino-8-(2,6-difluoro-phenyl)-4-(4-fluoro-2-methyl-phenyl)-8H-pyrido[2,3-d]pyrimidin-7-one (10 mg, 0.26 mmol) in 3 mL of tetrahydrofuran was added NaH (19 mg, 0.78 mmol). The mixture was stirred for 20 min at 23°, a soln of cyclopropanecarbonyl chloride (27 mg, 0.26 mmol) in tetrahydrofuran (1 mL) was added. The resulting mixture was heated to solvent reflux for 16 h to give the crude material, which was purified by preparative hplc to afford 25 mg (21%). LC-MS: 451.2 (MH+, m/z), 2.14 (Rt, min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07314881B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-228cd362a8c741b28adaa0209b78a2d0 |
| Source note | uspto-grants-2008_01 |