Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Methyl 3-methoxy-4-methyl-2-nitrobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Hydroxy-4-methyl-2-nitrobenzoic acid | HCID 81374 | — |
| 반응물 | Dichloromethane methanol | HCID 21226129 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 3-methoxy-4-methyl-2-nitrobenzoate | HCID 14543060 | 94.7% |
반응 단계
To a solution of 3-hydroxy-4-methyl-2-nitrobenzoic acid (365 g, 1.85 mol) in DMF (3280 mL) were added K2CO3 (524.4 g, 3.80 mol) and MeI (788 g, 5.55 mol) in one portion. Then the reaction mixture was stirred at room temperature overnight. TLC(CH2Cl2/MeOH=3:1) indicated the reaction was complete. Water (9 L) was added to the reaction mixture and the mixture was extracted with EtOAc (3 L×2). The combined organic layers were washed with 1 N aq. NaOH (1 L×2) and brine, dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound (395 g, 94.7%) as a light yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07998978B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-bc9a8d433be54c0487e702831b7e51a7 |
| 출처 메모 | uspto-grants-2011_08 |