関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 8-methylquinolin-2(1H)-one | HCID 5325167 | — |
| 生成物 | 2-Chloro-8-methylquinoline | HCID 21540195 | 63% |
反応手順
A mixture of 8-methyl-1H-quinolin-2-one (107) (580 mg, 3.6 mmol) and phosphorus oxychloride (5 mL) was stirred at 60° C. overnight. The mixture was then poured onto ice water and extracted with DCM (3×50 mL). The combined extracts were washed with water (2×100 mL) and dried with Na2SO4, and the solvent was removed. The residue was chromatographed on silica gel using 5% to 20% EtOAc in petroleum ether to give product (108) as small colorless crystals (400 mg, 2.3 mmol, 63% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08957073B2 |
|---|
| 出典データセット | uspto-grants-2015_02 |
|---|
| ORD ID | ord-79a3c70f3e354e5c8bbbeffcc8f0df80 |
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| 出典メモ | uspto-grants-2015_02 |
|---|
