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4,6-Dichloro-2-methyl-5-nitropyrimidine → (6-Chloro-2-methyl-5-nitro-pyrimidin-4-yl)(2,4,6-trimethyl-pyridin-3-yl)amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,6-Dichloro-2-methyl-5-nitropyrimidine | HCID 83192 | — |
| 反応物 | 2,4,6-Trimethyl-3-pyridinamine | HCID 98846 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (6-Chloro-2-methyl-5-nitro-pyrimidin-4-yl)(2,4,6-trimethyl-pyridin-3-yl)amine | HCID 10757155 | 36% |
反応手順
A solution of 2-methyl-5-nitro-4,6-dichloro-pyrimidine (208 mg, 1.00 mmol) in 2.5 ml of acetonitrile was treated with 2,4,6-trimethyl-3-amino-pyridine (273 mg, 2 mmol) stirred at room temperature 2 hours. The mixture was quenched with water and extracted with ethyl acetate. The organic layer was washed with brine, dried and concentrated to give red residue. The residue was purified through silica gel column chromatography using chloroform to 6% methanol in chloroform as eluent to give the title compound (110 mg, 36%) as an orange oil. 1H NMR (CDCl3) 68.78 (brs, 1H), 6.97 (s, 1H), 2.54 (s, 3H), 2.43 (s, 3H), 2.40 (s, 3H), 2.17 (s, 3H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07067664B1 |
| 出典データセット | uspto-grants-2006_06 |
| ORD ID | ord-87ad2dce7aaa4eb8a1514ad16a92702a |
| 出典メモ | uspto-grants-2006_06 |