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1,2-Dichloroethane → HCID 66571215、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Phenyl-piperidin-4-yl-methanol | HCID 339086 | — |
| 反応物 | 1-(4-fluorobenzyl)-1H-indole-2-carboxylic acid | HCID 18627069 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 66571215 | HCID 66571215 | 34.2% |
反応手順
The following was added sequentially to anhydrous DMF (5 mL): 1-(4-fluorobenzyl)-1H-indole-2-carboxylic acid (0.119 g, 0.443 mmol), Hunig's Base (0.232 ml, 1.329 mmol), EDC (0.093 g, 0.487 mmol), HOBT (0.075 g, 0.487 mmol), and phenyl(piperidin-4-yl)methanol (0.085 g, 0.443 mmol). The solution was stirred at room temperature for 30 h, at which time a 1:1 solution of EtOAc:Et2O was added and washed with 10% aq. Na2CO3. The organic solution was dried with MgSO4 and concentrated in vacuo to give a residue that was purified by silica gel chromatography (45 g silica, 80% EtOAc/Hexanes) to give 67 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846684B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-f43753a895c049a991e7334cb68c5904 |
| 出典メモ | uspto-grants-2014_09 |