関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 8-bromo-N-tert-butylquinazolin-2-amine | HCID 89781963 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 89782099 | HCID 89782099 | 85.7% |
反応手順
8-Bromo-N-(tert-butyl)quinazolin-2-amine (374a) (40 mg, 0.14 mmol) in THF (4 mL) at 0° C. was treated with NaH (60% dispersion in mineral oil, 8.6 mg, 0.21 mmol) and stirred at 0° C. for 30 min. MeI (10.71 μl, 0.17 mmol) was added and the solution was warmed to RT overnight (16 h). The reaction mixture was treated with brine and extracted with EtOAc (50 mL), dried over MgSO4, filtered and concentrated. Purification on a silica gel column (0-50% EtOAc in hexanes) afforded the title compound (34 mg, 0.12 mmol, 82% yield) as yellow viscous oil. m/z (ESI, +ve ion) 294.0/296.0 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09394297B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-6e79ecb1091b44bebf1f434691772157 |
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| 出典メモ | uspto-grants-2016_07 |
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