Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,3-Dihydro-1,4-benzodioxin-6-ol | HCID 9115273 | — |
| 촉매 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine | HCID 21624819 | 85% |
반응 단계
To a mixture of K2CO3 (47.54 g, 344 mmol) and Bu4NI (1.256 g, 3.4 mmol) in DMF was added 2,3-dihydro-benzo[1,4]dioxin-6-ol (26.2 g, 172 mmol) followed by iodomethane (16.1 ml, 258 mmol). After 16 hours the mixture was filtered. The solution was mixed with H2O and extracted with ethyl acetate. The combined organics were washed with brine, dried over MgSO4, filtered and concentrated in vacuo. Purification via flash chromatography (95:5 hexane/ethyl acetate) afforded methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine (24.23 g, 85%) as a clear oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846705B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-4e61b2e136dd4c8196edbfa0894d4da2 |
| 출처 메모 | uspto-grants-2014_09 |