関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | tert-Butyl 4-(((4-((4-bromo-2-fluorophenyl)amino)-6-methoxyquinazolin-7-yl)oxy)methyl)piperidine-1-carboxylate | HCID 11049999 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | Vandetanib | HCID 3081361 | 88.3% |
反応手順
37% Aqueous formaldehyde (3.5 ml, 42 mmol) was added to a solution of 4-(4-bromo-2-fluoroanilino)-7-(1-(tert-butoxycarbonyl)piperidin-4-ylmethoxy)-6-methoxyquinazoline (3.49 g, 6.22 mmol), (prepared as described for the starting material in Example 1), in formic acid (35 ml). After heating at 95° C. for 4 hours the volatiles were removed under vacuum. The residue was suspended in water and the mixture was adjusted to pH 10.5 by slow addition of a solution of 2N sodium hydroxide. The suspension was extracted with ethyl acetate. The organic layer was washed with brine, dried MgSO4 and evaporated to give 4-(4-bromo-2-fluoroanilino)-6-methoxy-7-(1-methylpiperidin-4-ylmethoxy)quinazoline (2.61 g, 88%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07173038B1 |
|---|
| 出典データセット | uspto-grants-2007_02 |
|---|
| ORD ID | ord-9fc48b1154c74828a455032b889f2591 |
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| 出典メモ | uspto-grants-2007_02 |
|---|
