Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 1-((4-Bromofuran-2-yl)methyl)-4-methylpiperazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-Methylpiperazine | HCID 53167 | — |
| 반응물 | 4-Bromo-2-furaldehyde | HCID 2757010 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-((4-Bromofuran-2-yl)methyl)-4-methylpiperazine | HCID 16099180 | — |
반응 단계
To a stirred mixture of 4-bromofuran-2-carbaldehyde (2.10 g, 12.0 mmol) and THF (10 mL) that was cooled in an ice bath was added 1-methylpiperazine (1.60 ml, 14.4 mmol) dropwise, followed by sodium triacetoxyborohydride (3.81 g, 18.0 mmol) in 3 portions as solid. Acetic acid (0.343 ml, 6.00 mmol) was added, and the reaction was stirred for 18 hours at ambient temperature. The dark mixture was diluted with water (10 mL) and basified to pH>12 by addition of 5N NaOH. The mixture was extracted with diethyl ether (3×50 mL). The combined organic phases were dried (Na2SO4), filtered, and concentrated in vacuo. The resulting black oil (2.10 g, 66%) was carried forward without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07723330B2 |
| 출처 데이터셋 | uspto-grants-2010_05 |
| ORD ID | ord-569affb3dc5d46d68f3789f3aab2719a |
| 출처 메모 | uspto-grants-2010_05 |