HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21110936, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | o-Xylyl bromide | HCID 6992 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 58885805 | HCID 58885805 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21110936 | HCID 21110936 | 47.5% |
Reaction Steps
To a mixture of (2R,6S)-4-[4-(6-Amino-5-hydroxy-pyridin-3-yl)-benzoyl]-2,6-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (100 mg, 0.23 mmol) and 1-bromomethyl-2-methyl-benzene (47 mg, 0.25 mmol) in DMF (2 mL) was added 2 M Cs2CO3 (0.35 mL, 0.7 mmol) followed by water (0.5 mL). The mixture was stirred at room temperature overnight. LCMS showed the reaction was completed, DMF was removed, followed by addition of 4 N HCl in dioxane (2 mL) and the reaction was stirred at room temperature for 3 hr. The volatiles were removed followed by addition of methanol. This solution was purified by prep-HPLC to afford {4-[6-Amino-5-(2-methyl-benzyloxy)-pyridin-3-yl]-phenyl}-(3,5-dimethyl-piperazin-1-yl)-methanone (47 mg, yield 46.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106197B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-4dd97b7ffae4474ea0f76af7779e135a |
| Source note | uspto-grants-2012_01 |