関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | HCID 178523802 | HCID 178523802 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Ferrate(4-), hexakis(cyano-C)-, tetrapotassium, (OC-6-11)- | HCID 11963580 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium Chloride | HCID 5234 | — |
| 生成物 | HCID 178509617 | HCID 178509617 | 43% |
反応手順
N-{trans-4-[(8-Bromoquinolin-4-yl)oxy]cyclohexyl}-3-fluorobenzamide (500 mg, 1.13 mmol) (see example 12), sodium carbonate (120 mg, 1.13 mmol) and palladium(II) acetate (13 mg, 0.06 mmol) were dissolved in N,N-dimethylacetamide (23 mL) and finely triturated potassium hexacyanoferrate (105 mg, 2.5 mmol) was added. The reaction mixture was stirred under a nitrogen atmosphere for 3 hours at 120° C. After cooling to room temperature, the reaction mixture was diluted with water and saturated sodium chloride solution and extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, then the sodium sulphate and solvent residues were removed. After chromatography of the residue, the desired product was obtained at 43% yield (190 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09428460B2 |
|---|
| 出典データセット | uspto-grants-2016_08 |
|---|
| ORD ID | ord-cd7c415faf06465e9aaab6efe123a5b2 |
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| 出典メモ | uspto-grants-2016_08 |
|---|
