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Bromine → Methyl 2-amino-5-bromonicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Methyl 2-aminopyridine-3-carboxylate | HCID 351633 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 2-amino-5-bromonicotinate | HCID 2763453 | 98.2% |
反応手順
Bromine (0.7 mL, 14 mmole) was added dropwise to a stirred solution of methyl 2-aminonicotinate (2.0 g, 13 mmole) in HOAc (50 mL). A suspension formed within 30 min. The reaction was allowed to stir at room temperature for 2 h, then was concentrated under vacuum. The residue was triturated with 1.0 N Na2CO3 (50 mL) and the solid was collected by suction filtration. The solid was washed with H2O (50 mL) and dried under vacuum to give the title compound (2.95 g, 98%) as a pale yellow solid: 1H NMR (400 MHz, CDCl3) δ 8.24 (d, J=2.5 Hz, 1H), 8.23 (d, J=2.5 Hz, 1H), 6.40 (br s, 2H), 3.90 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07879872B2 |
| 出典データセット | uspto-grants-2011_02 |
| ORD ID | ord-09e8d2d259f3418ca2ff14e7577761ff |
| 出典メモ | uspto-grants-2011_02 |