Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → Methyl 2-methoxy-3-methylbenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | 3-Methylsalicylic Acid | HCID 6738 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 생성물 | Methyl 2-methoxy-3-methylbenzoate | HCID 13229229 | 59.3% |
반응 단계
199.9 g (1.45 mol) of potassium carbonate is introduced into 1.5 l of dimethylformamide. At room temperature, 100 g (657.29 mmol) of 2-hydroxy-3-methylbenzoic acid, dissolved in 250 ml of dimethylformamide, is added in drops. After 30 minutes of stirring, 90 ml of methyl iodide is added in drops, and the batch is stirred overnight. The reaction mixture is added to ice water and extracted three times with methyl tert-butyl ether. The organic phases are washed with water and brine. After drying, the solvent is spun off, and the residue is chromatographed on silica gel (mobile solvent ethyl acetate/hexane). 70.21 g (59.3%) of the desired compound is isolated.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07662821B2 |
| 출처 데이터셋 | uspto-grants-2010_02 |
| ORD ID | ord-a4a327477158415db294da9e5cdfd606 |
| 출처 메모 | uspto-grants-2010_02 |