関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Amino-2-methylphenol | HCID 17818 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-Bromo-4-chloro-7H-pyrrolo[2,3-D]pyrimidine | HCID 45789827 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 5-(6-bromo-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)-2-methyl-phenol | HCID 69490164 | 70.3% |
反応手順
6-Bromo-4-chloro-7H-pyrrolo[2,3-d]pyrimidine (100 mg, 0.41 mmol), prepared as in reference 1, is mixed with 3-hydroxy-4-methylaniline (150 mg, 1.22 mmol) and diisopropylethylamine (213 μL, 1.22 mmol) in n-butanol (1.3 mL). The mixture is heated to 120° C. for 18 hours, with stirring. The reaction is then cooled to ambient temperature and the solvent is removed. The resultant crude product is purified by flash column chromatography using a gradient of 3-5% MeOH in DCM to yield 5-(6-bromo-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)-2-methyl-phenol (92 mg; 70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07253166B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-89414035e14542ca8ed3140ee143d449 |
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| 出典メモ | uspto-grants-2007_08 |
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