Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 3-(N,N-Diethylaminosulfonyl)-N-methoxy-N-methylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 3-(Diethylsulfamoyl)benzoic acid | HCID 794595 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-(N,N-Diethylaminosulfonyl)-N-methoxy-N-methylbenzamide | HCID 18375529 | 38.2% |
반응 단계
3-(N,N-diethylaminosulfonyl)benzoic acid (1.17 g, 4.55 mmol) and N,O-dimethylhydroxylamine hydrochloride (498 mg, 5.11 mmol) were dissolved in CH2Cl2 (30 mL). To this solution was added triethylamine (1.9 mL, 14 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (970 mg, 5.06 mmol) and 4-(N,N-dimethylamino)pyridine (117 mg, 0.958 mmol). The resulting solution was stirred at room temperature for 17 h then poured into saturated aqueous NaHCO3 and extracted 3× with ethyl acetate. The combined organics were washed with brine then dried over MgSO4 and concentrated under reduced pressure. The residue was purified by column chromatography (silica, 70:30 hexanes:acetone) to yield 522 mg of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06498165B1 |
| 출처 데이터셋 | uspto-grants-2002_12 |
| ORD ID | ord-d58cab61ebb845fb8c8419a52f6cd322 |
| 출처 메모 | uspto-grants-2002_12 |