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Potassium Carbonate → (R)-2-(2,5-dichloro-pyrimidin-4-ylamino)-3-methyl-butyramide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,5-Trichloropyrimidine | HCID 237259 | — |
| 反応物 | (R)-2-amino-3-methylbutanamide | HCID 444079 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (R)-2-(2,5-dichloro-pyrimidin-4-ylamino)-3-methyl-butyramide | HCID 86634077 | 62.4% |
反応手順
A mixture of (R)-2-amino-3-methyl-butyramide (50 mg), 2,4,5-trichloropyrimidine (67 mg) and K2CO3 (116 mg) in DMF (3 mL) was stirred at room temperature for 5 hr. The reaction mixture was diluted with DCM and washed with brine three times. The organic layer was dried with sodium sulfate and concentrated. The residue was purified by silica gel chromatography to provide 60 mg of (R)-2-(2,5-dichloro-pyrimidin-4-ylamino)-3-methyl-butyramide: 1H NMR (300 MHz, CDCl3) 8.2 (s, 1H), 6.2 (bs, 1H), 5.8 (bs, 1H), 5.6 (bs, 1H), 4.6 (dd, 1H), 2.4 (m, 1H), 1.2 (d, 6H). MS (m/e) 263 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08552186B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-ca9b4177ec1d419692fd65d148724ee5 |
| 出典メモ | uspto-grants-2013_10 |