Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetone → 1,3-Butanedione, 1-(2-furanyl)-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetone | HCID 180 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methyl 2-furoate | HCID 11902 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1,3-Butanedione, 1-(2-furanyl)- | HCID 12168 | 99.6% |
반응 단계
4.27 ml (5.04 g, 40 mmol) methyl 2-furoate was added to a suspension of NaH (made from 3.83 g commercial NaH slurry by removal of the mineral oil with pentane) in 30 ml anhydrous diethyl ether. To this was added, so as to maintain the temperature below 30° C., 5.87 ml (4.64 g, 80 mmol) acetone (dried over CaCl2). This mixture was heated under reflux for 2 h, cooled, and divided between diethyl ether and 3M HCl. The ether layer was washed with brine, dried (MgSO4), and concentrated to yield 6.06 g of a red oil (raw yield 99%) which was purified by vacuum distillation (b.p. 85°-90° C./1 torr).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05631374 |
| 출처 데이터셋 | uspto-grants-1997_05 |
| ORD ID | ord-8c764efa47ef4b9b8b9f366061dd03f4 |
| 출처 메모 | uspto-grants-1997_05 |