Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanesulfonamide → HCID 66667421, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanesulfonamide | HCID 72879 | — |
| 반응물 | 2-Methoxy-4-methylbenzoic acid | HCID 597164 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66667421 | HCID 66667421 | 63% |
반응 단계
2-Methoxy-4-methyl-benzoic acid (1.0 g. 6 mmol), methanesulphonamide (1.14 g. 12 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.31 g. 12 mmol), 4-dimethylaminopyridine (1.47 g. 12 mmol) and DCM (50 mL) were combined and stirred at room temperature under nitrogen for 18 hours. The reaction mixture was concentrated in vacuo and the residue suspended in water and acidified with aqueous potassium hydrogen sulphate (0.5 M). The mixture was extracted with EtOAc (1×30 mL). The organic layer was separated, washed with brine (2×20 mL), dried over sodium sulfate, filtered and evaporated to give a solid, which was triturated with hexane: diethyl ether (4:1) to yield the title compound as a white solid (0.92 g, 63%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09102621B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-a69f904eb1cb40979a7554961011bfd3 |
| 출처 메모 | uspto-grants-2015_08 |