関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Ethyl 3-ethoxy-2-propenoate | HCID 221780 | — |
| 反応物 | tert-Butyl 4-carbamothioylpiperidine-1-carboxylate | HCID 2735648 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | Ethyl 2-(piperidin-4-yl)-1,3-thiazole-5-carboxylate | HCID 86701983 | — |
反応手順
Ethyl 3-ethoxyacrylate (1.50 g, 10.38 mml) was dissolved in dioxane/water and chilled to −10° C. N-Bromosuccinimide (2.03 g, 11.42 mmol) was added and the mixture was stirred 1 hour at room temperature. tert-Butyl 4-carbamothioylpiperidine-1-carboxylate (2.54 g, 10.38 mmol) was added and the mixture was heated at 100° C. for 1 hour. The reaction mixture was poured into 25 mL saturated ammonium hydroxide and extracted with dichloromethane. The combined organic layers were washed with brine, dried with sodium sulfate, filtered, and concentrated. Normal phase chromatography provided the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09193723B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
|---|
| ORD ID | ord-ea33df414eef4f0ab07f324266e29870 |
|---|
| 出典メモ | uspto-grants-2015_11 |
|---|
