HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-[(5-Fluoro-2-{[4-(hydroxymethyl)phenyl]amino}-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide → HCID 57974221, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-[(5-Fluoro-2-{[4-(hydroxymethyl)phenyl]amino}-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide | HCID 57974211 | — |
| Catalyst | Manganese dioxide | HCID 14801 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57974221 | HCID 57974221 | 96.1% |
Reaction Steps
A 50-mL of round bottom flask was charged with 2-[(5-fluoro-2-{[4-(hydroxymethyl)phenyl]amino}-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide (200 mg, 0.5 mmol, 1.0 eq) and dioxane (20 mL). MnO2 (217 mg, 2.5 mmol, 5.0 eq) was added slowly to this solution. Upon completion of the addition, the reaction mixture was heated at reflux for 16 h. The reaction mixture was filtered through celite and the solvent was evaporated to produce the desired product (189 mg, 48% yield) which was found to be 82% pure by HPLC. MS: M(C21H20FN5O2)=393.42, (M+H)+=394. This crude material was used for next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07884098B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-edfc2c172778420583974c34750f615c |
| Source note | uspto-grants-2011_02 |