HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 86732402, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 86732403 | HCID 86732403 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86732402 | HCID 86732402 | — |
Reaction Steps
Cesium carbonate (265 mg, 0.82 mmol) and methyl idodide (51 μL, 0.82 mmol) are added to a solution of 4-(2,5-dioxo-1-(2-(trifluoromethyl)pyridin-4-yl)-1,2,3,4,5,6,7,8-octahydroquinazolin-4-yl)-3-(methylsulfonyl)benzonitrile (example 57, 200 mg, 0.41 mmol) in N,N-dimethylformamide (3 mL), and the mixture is stirred at room temperature for 2 h. Ethyl acetate is added, and the mixture is extracted three times with water. The organic phase is dried over Mg2SO4 and concentrated under reduced pressure. The residue is it) purified by flash chromatography on silica (gradient dichloromethane/methanol 99:1 to 97:3). Yield: 134 mg; ESI mass spectrum [M+H]+=505; Retention time HPLC: 0.60 min (X012_S02).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115093B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-de4f20aa68dc4412a4c44eed80f580e5 |
| Source note | uspto-grants-2015_08 |