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Sodium Hydroxide → 3-Amino-6-bromo-5-(trifluoromethyl)picolinic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 3-amino-6-bromo-5-(trifluoromethyl)picolinate | HCID 58964428 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Amino-6-bromo-5-(trifluoromethyl)picolinic acid | HCID 58442350 | — |
反応手順
3-Amino-6-bromo-5-trifluoromethyl-pyridine-2-carboxylic acid methyl ester (1.40 g, 4.68 mmol) was suspended in MeOH (15 ml); Sodium hydroxide (2.0 M aqueous solution) (14.04 ml, 28.1 mmol) was added and the suspension was stirred at RT overnight. The mixture was concentrated in vacuo and the resulting residue was dissolved in water (100 ml) and then acidifed by the addition of 5.0M HCl(aq). The product was extracted into ethyl acetate (2×75 ml) and the combined organic extracts were washed with water (50 ml), brine (25 ml), dried (MgSO4) and concentrated in vacuo to afford the title product as a yellow solid. 1H-NMR: [400 MHz, DMSO-d6, δH 13.24 (1H, br s, CO2H), 7.74 (1H, s, ArH), 7.17 92H, br s ArN H2). m/z 285.1, 287.1 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08476269B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-81eeffc9092544f0a7711769ee870cc6 |
| 出典メモ | uspto-grants-2013_07 |