HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68569120, compound → HCID 10322398, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68569120 | HCID 68569120 | — |
| Reactant | 2-Chloro-4-[1-methyl-3-(4-methylphenyl)-1H-pyrazol-4-yl]pyrimidine | HCID 71379188 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 10322398 | HCID 10322398 | — |
Reaction Steps
3-(1-Methyl-piperidin-4-ylmethoxy)-phenylamine dihydrochloride (206 mg, 0.7 mmol) is suspended in 1.5 mL n-butanol and 1.5 mL dioxane. 2-Chloro-4-(1-methyl-3-p-tolyl-1H-pyrazol-4-yl)-pyrimidine (100 mg, 0.35 mmol) is added and the mixture heated under reflux for 15 h. The yellow suspension is evaporated to dryness and the residue portioned between 8 mL 20% potassium carbonate solution and 10 mL dichloromethane. The organic phase is dried with sodium sulfate and evaporated. The crude product is purified by flash-chromatography on Silica Gel using dichloromethane/methanol 100:1.25→100:5 and then dichloromethane/methanol/conc. ammonia 100:5:0.25→100:10:0.25. The title compound is obtained as a foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07691855B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-59138146c69e4073ad4cbd505887b35a |
| Source note | uspto-grants-2010_04 |