Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2-amino-2-methyl-N-(methylsulphonyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | Methanesulfonamide | HCID 72879 | — |
| 반응물 | 2-Amino-3-methylbenzoic acid | HCID 78101 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-amino-2-methyl-N-(methylsulphonyl)benzamide | HCID 86660264 | — |
반응 단계
20 g (128 mmol) of 2-amino-3-methylbenzoic acid are dissolved in 600 ml of dichloromethane, and 10.98 g (115 mmol) of methanesulphonamide, 24.40 g (154 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 15.68 g (128 mmol) of 4-(dimethylamino)pyridine are then added under argon. The reaction is stirred at room temperature for 16 h, the solvent is distilled off and the residue is taken up in ethyl acetate and water. The ethyl acetate phase is washed four times with a 1N hydrochloric acid solution and then in each case once with water and a concentrated sodium chloride solution. After drying over sodium sulphate, the desired product is obtained by chromatographic purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08658800B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-309219c488304383992fdc092b007281 |
| 출처 메모 | uspto-grants-2014_02 |