Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dimethyl-3-nitrobenzene → 6-Methyl-2-nitrophenylpyruvic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dimethyl-3-nitrobenzene | HCID 6739 | — |
| 반응물 | Diethyl Oxalate | HCID 7268 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-Methyl-2-nitrophenylpyruvic acid | HCID 21194232 | 61% |
반응 단계
Sodium (3.802 g, 165.38 mmol, 2.5 eq) was added portionwise into ethanol (66 mL, 1M) at 0° C. Next, 3-nitro-ortho-xylene (10.00 g, 66.15 mmol, 1 eq) and diethyl oxalate (19.33 g, 132.23 mmol, 2 eq) were added. The mixture was stirred at room temperature for 18 hours and then refluxed for 10 minutes. 1N sodium hydroxide and water were added and the reaction was stirred for one hour. The ethanol was removed under vacuum. Water was added and the aqueous solution was acidified with concentrated hydrochloric acid to ph~2. The mixture was extracted with methylene chloride. The extracts were dried (magnesium sulfate) and concentrated to give the title compound (9.0 g, 61%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05616591 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-631527924b8e4da9a6a90a47ed6c1ba9 |
| 출처 메모 | uspto-grants-1997_04 |