Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Citric Acid → Methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Citric Acid | HCID 311 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Methyl Anthranilate | HCID 8635 | — |
| 반응물 | 2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate | HCID 86676334 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | Methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate | HCID 71238679 | 92.2% |
반응 단계
To a mixture of 2.09 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate and 20 mL of methylene chloride were added 982 mg of methyl 2-aminobenzoate and 2.10 mL of pyridine under ice-cooling, followed by stirring at room temperature for 15 hours. To the reaction mixture was added a 10% aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 2.61 g of methyl 2-{[(3-{[2-(trimethylsilyl)ethoxy]carbonyl}phenyl)sulfonyl]amino}benzoate as a colorless oily substance.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09284295B2 |
| 출처 데이터셋 | uspto-grants-2016_03 |
| ORD ID | ord-85f77c7d02fa4c4e97559078b7e23ae5 |
| 출처 메모 | uspto-grants-2016_03 |