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Triethylamine → (r)-2-(2-Chloro-5-ethyl-pyrimidin-4-ylamino)-3-methyl-butan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | D-Valinol | HCID 6950587 | — |
| 反応物 | 2,4-Dichloro-5-ethylpyrimidine | HCID 10012458 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (r)-2-(2-Chloro-5-ethyl-pyrimidin-4-ylamino)-3-methyl-butan-1-ol | HCID 58727632 | 60.9% |
反応手順
A solution of 882 mg (5.0 mmol) of 2,4-Dichloro-5-ethyl-pyrimidine and 0.75 ml (5.5 mmol) triethylamine in 5 ml of acetonitrile is mixed with 672 mg (6.5 mmol) of (R)-2-Amino-3-methyl-butan-1-ol. The batch is stirred at room temperature for 16 hours and is finally concentrated by evaporation. The remaining residue is purified by chromatography (DCM/EtOH 90:10). 742 mg of the product is obtained that still contains considerable amounts of (R)-2-Amino-3-methyl-butan-1-ol. The material is used without further purifications.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456191B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-96657b3df174497b88da192d1bcc721a |
| 出典メモ | uspto-grants-2008_11 |