Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Bromide → 3,4-Dihydroxy-5-nitrobenzaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Bromide | HCID 260 | — |
| 반응물 | 5-Nitrovanillin | HCID 81134 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3,4-Dihydroxy-5-nitrobenzaldehyde | HCID 5748957 | — |
반응 단계
17.1 g of 4-hydroxy-3-methoxy-5-nitrobenzaldehyde are treated with 170 ml of constant-boiling hydrobromic acid and heated under reflux for 3.5 hours. After cooling the separated precipitate is filtered under suction, washed twice with ice-water and taken up in ethyl acetate. The organic phase is washed twice with 50 ml of sodium chloride solution each time, dried over magnesium sulfate and evaporated in a water-jet vacuum. The crystals obtained are taken up in methylene chloride, whereupon the solution is filtered over a ten-fold amount of silica gel. The material obtained is crystallized from ethyl acetate/isopropyl ether. There is obtained 3,4-dihydroxy-5-nitrobenzaldehyde in the form of yellow crystals of m.p. 142°-143°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05389653 |
| 출처 데이터셋 | uspto-grants-1995_02 |
| ORD ID | ord-abb4814a8f9b43979a8172da63570498 |
| 출처 메모 | uspto-grants-1995_02 |