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Triethylamine → 1-(Benzo[1,2,3]thiadiazole-5-carbonyl)-piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | 1,2,3-Benzothiadiazole-5-carboxylic acid | HCID 2735458 | — |
| 反応物 | 4-Piperidone hydrochloride | HCID 3084851 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(Benzo[1,2,3]thiadiazole-5-carbonyl)-piperidin-4-one | HCID 22397465 | 29.5% |
反応手順
CDI (4.5 g) added to a solution of the benzo[1,2,3]thiadiazole-5-carboxylic acid (5 g) stirring in THF (100 ml) at RT. After 1 hour 4-piperidone hydrochloride (3.7 g) and triethylamine (4.3 ml) were added and the mixture stirred overnight. The resulting mixture was diluted with ethyl acetate, washed with 2M HCl (100 ml), saturated NaHCO3 solution (200 ml) and then with saturated brine (200 ml). The organic layer was dried (MgSO4) and evaporated to leave a residue which was purified by column chromatography (silica, eluting with mixtures of ethyl acetate in dichloromethane) to give the product as a yellow oil (2.1 g; MS: APCI+(M+H)262).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07238811B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-5cbbd9b1003a49f3a3a7bfa41754bdf2 |
| 出典メモ | uspto-grants-2007_07 |