関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chloro-2-methylphenyl isocyanate | HCID 142157 | — |
| 反応物 | HCID 68903795 | HCID 68903795 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 11648354 | HCID 11648354 | 83.3% |
反応手順
4-Chloro-1-isocyanato-2-methyl-benzene (93.3 mg, 0.56 mmol) was added to a solution of (4-Amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(5-amino-pyridin-3-yl)-methanone (150 mg, 0.51 mmol) in pyridine (5 mL). The mixture was heated to 45° C. for 12 h. The reaction mixture was concentrated in vacuo and the resulting yellow solid was triturated with CH2Cl2, filtered, and washed with CH2Cl2. Purification by flash column chromatography [(10% NH4OH/MeOH)/ethyl acetate 2:98] afforded the title compound as a white solid (197 mg, 83%). MS: 464.1 (MH+); HPLC Rf: 5.55 min. (HPLC method 4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07595325B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-2005108721c4467896be0ffb4794ac91 |
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| 出典メモ | uspto-grants-2009_09 |
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