Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione 9-(1,2-dimethylethylene) acetal
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione | HCID 19035976 | — |
| 용매 | 2,3-Butanediol | HCID 262 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione 9-(1,2-dimethylethylene) acetal | HCID 67722801 | 78.5% |
반응 단계
A suspension of 9H-indeno[1,2-b]pyrazine-3,9(4H)-dione (2.0 g, 10.09 mmol) in toluene (50 ml), 2,3-butanediol (20 ml) and p-toluenesulfonic acid (40 mg) was refluxed with water separation for 20 hours. The reaction mixture was evaporated in vacuo to dryness and another portion of toluene, 2,3-butanediol and p-toluenesulfonic acid was added and the mixture was refluxed again for 20 hours. After evaporation to dryness, the residue was suspended in ethanol (10 ml) and the precipitate was filtered off and washed with ethanol and dried to give 2.14 g (78.5%) of the title compound as a mixture of isomers. 1H-NMR (DMSO-d6, δ): 1.24-1.4 (m, 6H), 4.03-4.87 (m, 2H), 7.42-7.91 (m, 5H), 12.6 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468748 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-5e780d7eccc2441cbdaede3581cdc59d |
| 출처 메모 | uspto-grants-1995_11 |