Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1525643생성일: 2026년 10월 26일
Potassium Carbonate → 4-{[3-Chloro-4-(trifluoromethyl)phenoxy]methyl}-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide
https://huagongshe.com/reaction/1525643
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Chloro-4-(trifluoromethyl)phenol | HCID 13609147 | — |
| 반응물 | 4-(Bromomethyl)-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide | HCID 89619586 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-{[3-Chloro-4-(trifluoromethyl)phenoxy]methyl}-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide | HCID 71616020 | 10.3% |
반응 단계
To a solution of 4-(bromomethyl)-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide (Preparation 1, 167 mg, 0.47 mmol) in dimethylsulfoxide (2 mL) was added 2-chloro-4-hydroxybenzotrifluoride (92 mg, 0.47 mmol) followed by addition of potassium carbonate (129 mg, 0.94 mmol). The reaction was left to stir at room temperature for 18 hours. The reaction was diluted with dichloromethane (20 mL) and washed with aqueous potassium hydrogen sulfate (5 mL). The organic phase was separated and the aqueous phase extracted with dichloromethane (2×20 mL). The combined organic layers were washed with brine (30 mL) and filtered through a phase separation cartridge. The solvent was removed under reduced pressure and the crude product purified by reverse phase preparative HPLC. The correct fractions were combined and reduced to dryness to afford the title compound as white solid (23 mg, 10%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09085517B2 |
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| 출처 데이터셋 | uspto-grants-2015_07 |
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| ORD ID | ord-2a9cf24699f942f9afe515c5343ee0f8 |
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| 출처 메모 | uspto-grants-2015_07 |
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