関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-[3-Chloro-4-(3-fluoro-benzyloxy)-phenylamino]-6-nitro-quinazoline | HCID 53630476 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Allitinib metabolite M6 | HCID 53630477 | 61% |
反応手順
In a flask equipped with a reflux condenser, the compound obtained in Example 6 1.60 g (3.77 mmol), reduced iron powder 1.05 g (18.85 mmol, 5 eq), glacial acetic acid (2 mL) and methanol (40 mL) were mixed. The mixture was refluxed in an oil bath at a temperature of 85° C. for 2.5 h. Then the iron powder was filtered of, the filtrate was diluted with ethyl acetate, washed sequentially with NaHCO3 solution and water. The organic phase was dried and concentrated to obtain yellow solid, which was identified as the title compound. Yield: 61%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08044063B2 |
|---|
| 出典データセット | uspto-grants-2011_10 |
|---|
| ORD ID | ord-4858870967fe4189a60da34c0b585ad0 |
|---|
| 出典メモ | uspto-grants-2011_10 |
|---|
