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Potassium Carbonate → N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Trimethylbenzeneacetyl chloride | HCID 11030754 | — |
| 反応物 | 4-Amino-1-ethoxy-piperidine-4-carbonitrile | HCID 59614603 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide | HCID 59614586 | 89.5% |
反応手順
3.0 g of (2,4,6-trimethyl-phenyl)-acetyl chloride and 10 g of potassium carbonate in 90 ml of acetonitrile were treated at 0° C. with a solution of 3.6 g of 4-amino-1-ethoxy-piperidine-4-carbonitrile in 30 ml of acetonitrile. After stirring for 18 hours at room temperature the reaction mixture was poured into 100 ml of ice water and extracted with ethyl acetate. The organic phase was washed with brine and concentrated. Chromatography (heptane/ethyl acetate 5:1) yielded 4.5 g of N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide as a solid, mp: 194-195° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08415369B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-2cf93ac1b11c47c39308d7baaf7c629b |
| 出典メモ | uspto-grants-2013_04 |