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Methylamine → 3-iodo-N,4-dimethylbenzamide
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-Iodo-4-methylbenzoyl chloride | HCID 17752157 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-iodo-N,4-dimethylbenzamide | HCID 19688440 | 95% |
反応手順
To a cooled (0° C.) solution of 3-iodo-4-methylbenzoyl chloride (2.80 g; 10.0 mmol) in DCM (10 mL) was slowly added a 2 M solution of methylamine in THF (11 mL, 2.2 eq.). Upon completion of the addition, the ice bath was removed and the mixture was stirred overnight. All volatiles were removed in vacuo and the residue was treated with aq. NaHCO3 (25 mL) and subsequently extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4 and evaporated. The target compound 3-iodo-N,4-dimethylbenzamide (2.62 g, 95% yield) was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642611B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-4d373b660c0a44c5833c706f21fb3554 |
| 出典メモ | uspto-grants-2014_02 |