関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 3-Iodobenzoic acid | HCID 12060 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-iodo-N-methylbenzamide | HCID 3384366 | — |
反応手順
To a solution of 3-iodobenzoic acid (1.5 g, 6 mmol) in anhydrous DMF (10 mL) was added 1,1′-carbonyldiimidazole (1.2 g, 7.2 mmol). The reaction mixture was heated to 50° C. under an atmosphere of nitrogen for 1 h. Upon cooling to room temperature, a solution of methylamine in THF (2 M, 6 mL, 10 mmol) was added. The reaction was stirred at r.t. for 15 min and then transferred into a solution of cold, saturated ammonium chloride (200 mL). The resulting precipitate was collected by filtration and dried to afford the title compound as a white solid, mp 94-97° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08765779B2 |
|---|
| 出典データセット | uspto-grants-2014_07 |
|---|
| ORD ID | ord-c78de95eccbc4fe885be31529264c23d |
|---|
| 出典メモ | uspto-grants-2014_07 |
|---|
