関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Amino-2-chloropyridine | HCID 79305 | — |
| 反応物 | 2-Bromo-5-methylbenzoic acid | HCID 228080 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 2-(6-Chloropyridin-3-ylamino)-5-methylbenzoic acid | HCID 86657254 | 46% |
反応手順
A mixture of 6-chloropyridin-3-amine (11.67 mmol, 1.5 g) and 2-bromo-5-methylbenzoic acid (23.34 mmol, 5.02 g), Cu (1.17 mmol, 0.1 g), Cu2O (0.58 mmol, 0.1 g) and K2CO3 (23.34 mmol, 3.2 g) in 1,2-dimethoxyethane (15 ml) was heated at 130° C. for 16 hours, under argon atmosphere. Water was added and the mixture was filtered through celite. HCl 2N aqueous solution was added until pH 6 and the solid formed was filtered off. The crude was purified by chromatography eluting with DCM/MeOH mixtures affording 1.40 g (yield 46%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536165B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ed1c3d76e4334931a3392edaa263a26b |
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| 出典メモ | uspto-grants-2013_09 |
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