関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentane | HCID 8003 | — |
| 反応物 | Ethyl 2-aminothiazole-4-carboxylate | HCID 73216 | — |
| 反応物 | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-((tert-butoxycarbonyl)amino)-1,3-thiazole-4-carboxylate | HCID 22280595 | 66.4% |
反応手順
Ethyl 2-aminothiazole-4-carboxylate 87 (10.0 g, 58.1 mmol) was taken up in 150 mL of anhydrous THF along with di-tert-butyl carbonate (12.67 g, 58.1 mmol) and 4-(dimethyl)aminopyridine (DMAP) (10 mg, 0.082 mmol). The reaction mixture was stirred at 50° C. for 4 h and then at room temperature for 18 h. It was then concentrated under reduced pressure to obtain a thick oil. Pentane was added and the resulting crystalline materials were collected by filtration and dried to afford 88 (10.5 g, 66% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09326986B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
|---|
| ORD ID | ord-a3d6ca76c1374673babeeba4ad81903f |
|---|
| 出典メモ | uspto-grants-2016_05 |
|---|
