Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,5-Dihydroxybenzoic acid → 4-(3-Methoxycarbonyl-4-methoxyphenoxy)-1-nitrobenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,5-Dihydroxybenzoic acid | HCID 3469 | — |
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 5-(4-Nitrophenoxy)-salicylic acid | HCID 21492504 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 4-(3-Methoxycarbonyl-4-methoxyphenoxy)-1-nitrobenzene | HCID 23023095 | — |
반응 단계
To a solution of 4-(3-carboxy-4-hydroxyphenoxy)-1-nitrobenzene (prepared from 2,5-dihydroxybenzoic acid in a manner analogous to that described in Method A13, Step 1, 12 mmol) in acetone (50 mL) was added K2CO3 (5 g) and dimethyl sulfate (3.5 mL). The resulting mixture was heated at the reflux temp. overnight, then cooled to room temp. and filtered through a pad of Celite®. The resulting solution was concentrated under reduced pressure, absorbed onto SiO2, and purified by column chromatography (50% EtOAc/50% hexane) to give 4-(3-methoxycarbonyl-4-methoxyphenoxy)-1-nitrobenzene as a yellow powder (3 g): mp 115-118° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841330B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-bb3abe07a2b04f53bf762bd6d2d10bed |
| 출처 메모 | uspto-grants-2014_09 |