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Sodium hydride → HCID 178422579、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Cyclohexane-1,1-diol | HCID 19352763 | — |
| 反応物 | 5-Chloro-7-(4-dimethylamino-3-methylphenyl)-[1,6]naphthyridine | HCID 44632882 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | HCID 178422579 | HCID 178422579 | — |
反応手順
200 mg (1.7 mmol) cyclohexanediol was placed in 1.5 ml dimethylacetamide and 47 mg (1.17 mmol) sodium hydride (60%) were added and the mixture was stirred for 15 min at ambient temperature. Then 100 mg (0.31 mmol) 6.1 was added and the mixture was stirred for 2 h at 70° C. The reaction mixture was diluted with dichloromethane and extracted 1× with water. The organic phase was dried with MgSO4 and evaporated down. The residue was purified by chromatography (RP-HPLC-MS). The corresponding fractions were freeze-dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08957088B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-42b90fdd55b24797830070f38b54fa4e |
| 出典メモ | uspto-grants-2015_02 |