Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl acetoacetate → 3-Isopropenyl-4-nitro-2(3H)-benzimidazolone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl acetoacetate | HCID 7757 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 3-Nitro-1,2-phenylenediamine | HCID 4359525 | — |
| 반응물 | Methanol--water (1/1) | HCID 22242641 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 3-Isopropenyl-4-nitro-2(3H)-benzimidazolone | HCID 10536836 | — |
반응 단계
0.3 ml of 47% potassium hydroxide and then 115 mmol of methyl acetoacetate are added to 100 mmol of 2-amino-3-nitroaniline in 50 ml of xylene brought to 120° C. The whole mixture is brought to reflux for 4 hours and the water/methanol mixture formed is removed by means of a Dean and Stark apparatus. 18 ml of 47% potassium hydroxide and 200 ml of water are then added. The aqueous phase is washed with xylene, brought to pH=6 with 12N hydrochloric acid and then extracted with ethyl acetate and the expected product is purified by chromatography on a silica column, using a dichloromethane/methanol (95/5) mixture as eluent.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05652246 |
| 출처 데이터셋 | uspto-grants-1997_07 |
| ORD ID | ord-f50582cc8b924b648e0fe750673e8523 |
| 출처 메모 | uspto-grants-1997_07 |