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Sodium hydride → 8-(6-Benzyloxy-pyridin-2-yl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(Benzyloxy)-6-fluoropyridine | HCID 57753871 | — |
| 反応物 | 2-(4-(Trifluoromethoxy)phenyl)-2,8-diazaspiro[4.5]decan-1-one | HCID 66742759 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 8-(6-Benzyloxy-pyridin-2-yl)-2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one | HCID 56655756 | 73% |
反応手順
To a suspension of NaH (9 mg, 0.24 mmol) in DMF (1 mL) at 0° C. was added a solution of 2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decan-1-one (described in example 1 step C, 50 mg, 0.16 mmol) and stirring was continued for 30 mins. A solution of 2-benzyloxy-6-fluoro-pyridine (39 mg, 0.19 mmol) in DMF (0.5 mL) was added and the mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with ethyl acetate and washed with brine, 1N HCl and again with brine. The organic phase was dried (Na2SO4), filtered and evaporated under reduced pressure to yield the title compound as a light yellow solid (58 mg, 73%). MS (ESI): 498.2 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08552024B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-4b1db75e31b74de59f74fb22e6937149 |
| 出典メモ | uspto-grants-2013_10 |