Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-(o-Tolyl)piperazine dihydrochloride | HCID 91964 | — |
| 반응물 | 4-Fluoro-2-methyl-5-nitrobenzoic acid | HCID 22313101 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid | HCID 89690648 | — |
반응 단계
To a stirred solution of 4-fluoro-2-methyl-5-nitro-benzoic acid (5.0 g, 25.10 mmol) in anhydrous DMF (100 mL), potassium carbonate (10.4 g, 75.3 mmol) was added under N2 atmosphere followed by 1-o-tolyl-piperazine 2 HCl (8.13 g, 32.6 mmol). The reaction mixture was allowed to stir at room temperature overnight. The progress of the reaction was checked by TLC, upon completion of the reaction, solvent was removed in vacuo. The residue obtained was acidified with conc. HCl (≈pH=2-3). Yellow solid obtained was filtered and washed with water (3×75 mL), diethyl ether and dried under vacuo to obtain the pure product 2-methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid. Yield (6.5 g, 73%; and yellow solid).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09409897B2 |
| 출처 데이터셋 | uspto-grants-2016_08 |
| ORD ID | ord-ed984582d8f44b28aed168943abd906e |
| 출처 메모 | uspto-grants-2016_08 |