Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-bromo-N-(2-methylbut-3-yn-2-yl)benzenamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Bromoaniline | HCID 7807 | — |
| 반응물 | 1-Butyne, 3-chloro-3-methyl- | HCID 70679 | — |
| 촉매 | Copper | HCID 23978 | — |
| 촉매 | Cuprous chloride | HCID 62652 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 4-bromo-N-(2-methylbut-3-yn-2-yl)benzenamine | HCID 20082271 | — |
반응 단계
To a solution of 4-bromobenzenamine (4.0 g, 23 mmol), TEA (4.3 ml, 31 mmol), 2.0 ml of water, copper (0.058 g, 0.91 mmol) and copper(I) chloride (0.058 g, 0.59 mmol) in diethyl ether (9.8 ml, 20 mmol) was added 3-chloro-3-methylbut-1-yne (2.0 g, 20 mmol), dropwise. After stirring overnight, the reaction mixture was transferred to a seperatory funnel containing water and diethyl ether. The aqueous layer was washed 3× with EtOAc. The organic layers were combined, dried with MgSO4, filtered and concentrated. The crude oil was purified with by MPLC (100% DCM to 10% (91/10/1 DCM:MeOH:NH4OH)) to provide the product as an oil. MS m/z: 240 (M+2).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745484B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-84f384e1b4ca4b4897235a5af4920794 |
| 출처 메모 | uspto-grants-2010_06 |