Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-Bromo-N-(3-iodo-phenyl)-butyramide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Iodoaniline | HCID 12271 | — |
| 반응물 | 4-Bromobutyryl chloride | HCID 70225 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Cyclohexane | HCID 8078 | — |
| 생성물 | 4-Bromo-N-(3-iodo-phenyl)-butyramide | HCID 86678177 | 64% |
반응 단계
To a solution of 3-iodoaniline (1.5 g, 6.85 mmol) and triethylamine (1.34 mL, 9.59 mmol) in dichloromethane (28 mL) at 0° C. was added dropwise 4-bromobutyryl chloride (0.99 mL, 8.56 mmol). The reaction mixture was then stirred at room temperature overnight. The organic extract was washed with an aqueous 1M HCl solution, aqueous 1M NaOH solution and brine, dried (Na2SO4), filtered, concentrated under vacuum. The crude residue was purified by silica gel column chromatography using a gradient of EtOAc (0-15%) in cyclohexane to yield a sticky solid. Trituration in a mixture of cyclohexane and ether and then filtration give the title compound as a solid (1.61 g, 64%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846712B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-f7871a57384f4a538967d51a3894c02f |
| 출처 메모 | uspto-grants-2014_09 |