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Water → Ethyl 4-[(2-methylbenzoyl)amino]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzocaine | HCID 2337 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Methylbenzoyl chloride | HCID 70276 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 4-[(2-methylbenzoyl)amino]benzoate | HCID 689910 | 77.4% |
反応手順
A mixture of 43.42 g (0.26 mol) of ethyl 4-aminobenzoate and 40.8 g (0.26 mol) of 2-methylbenzoyl chloride in 150 ml of dichloromethane is cooled in an ice bath and 26.56 g (0.26 mol) of triethylamine is added dropwise. After the addition, the solution is stirred at room temperature overnight. The mixture is poured into water and the organic layer separated. The organic layer is washed with water, 1N HCl, 1M NaHCO3 and dried (Na2SO4). The solvent is removed and the solid slurried with ethyl acetate and filtered to give 57 g of ethyl 4-[(2-methylbenzoyl)amino]benzoate as crystals, m.p. 110°-115° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05869483 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-592d5fcdb688449bb329269df607bd14 |
| 出典メモ | uspto-grants-1999_02 |