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, and dimethoxyacetal (35 ml) and a catalytic amount of p-toluenesulfonic acid were added thereto, followed by heating at reflux for 6 hours. After being allowed to stand for cooling, the mixture was adjusted to alkaline with an aqueous solution of sodium hydroxide, followed by extraction with ether. The organic layer was washed with a saturated saline and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=99/1) to give Compound IIbk-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-b56b9681518f4d3ebb66dfcc047e363d |
| 출처 메모 | uspto-grants-2003_02 |