Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
p-Toluenesulfonic acid → 4-Methoxy-2,2-dimethyl-1,3-benzodioxole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 3-Methoxycatechol | HCID 13622 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | 4-Methoxy-2,2-dimethyl-1,3-benzodioxole | HCID 15061094 | — |
반응 단계
3-methoxycatechol (25 g) was dissolved in benzene, mixed with dimethoxyacetal (35 ml) and a catalytic amount of tosylic acid, and then, heat-refluxed for 6 hours. The resultant was allowed to stand for cooling, alkalified by adding an aqueous sodium hydroxide solution, and extracted with ether. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over manganese sulfate, and evaporated under reduced pressure for removing the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=99/1) to give Compound IIbv-a (19.4 g, 60.5%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06514996B2 |
| 출처 데이터셋 | uspto-grants-2003_02 |
| ORD ID | ord-6333eb2aab974270b8b7deba206c7a2b |
| 출처 메모 | uspto-grants-2003_02 |