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Naphthyridinone → 9-(4-Chlorophenyl)-8-(2,4-dichlorophenyl)-2,4,4,6-tetramethyl-4,6-dihydro-5H-[1,3]oxazino[5,4-c]-1,8-naphthyridin-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Naphthyridinone | HCID 11386747 | — |
| 反応物 | HCID 178418689 | HCID 178418689 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-(4-Chlorophenyl)-8-(2,4-dichlorophenyl)-2,4,4,6-tetramethyl-4,6-dihydro-5H-[1,3]oxazino[5,4-c]-1,8-naphthyridin-5-one | HCID 11364268 | — |
反応手順
To the product of Example 1 (59.5 mg) in THF (2 mL) at 0° C. was added 0.52 mL MeMgBr solution (1.4 M, 75% toluene/25% THF). After 10 min the reaction was quenched with saturated aqueous NH4Cl and then diluted with EtOAc. The solution was washed with 10% aqueous NaHSO4 followed by aqueous NaHCO3/NaOH (4:1) before drying (Na2SO4). The concentrated residue was purified by preparative TLC (silica gel) eluted with 15% EtOAc in hexane affording the title compound. HPLC/MS: 512.0 (M+1), 514.0 (M+3); Rt=5.14 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728141B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-1c35074f7fe847f8b31359431c209c52 |
| 出典メモ | uspto-grants-2010_06 |