関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cyclohexanol | HCID 7966 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-7-(phenylmethyl)-7H-pyrrolo[2,3-d]pyrimidine | HCID 15185356 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7-Benzyl-4-cyclohexyloxy-7H-pyrrolo[2,3-d]pyrimidine | HCID 22484555 | 59% |
反応手順
To a flame dried flask under nitrogen was charged 84 mg (2.10 mmol) of 60% sodium hydride in mineral oil and 3.0 mL of THF and the mixture cooled to 0° C. Cyclohexanol (0.18 mL/1.70 mmol) was added and the reaction mixture stirred for 5 min. A solution of 102 mg (0.419 mmol) of the product from Method L in 1.0 mL of THF was added and the mixture heated to reflux for 3 h. After cooling to room temperature, the reaction mixture was acidified to pH 1 with 2 N HCl and concentrated in vacuo. The resulting residue was then slurried in ethyl acetate, filtered and the filtrate concentrated in vacuo to provide 76 mg (59%) of the title compound as an oil. LRMS: 308 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06610847B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-1af6729f32d649eb86ec7855e7a28507 |
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| 出典メモ | uspto-grants-2003_08 |
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