Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 5-Amino-2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Methallyl alcohol | HCID 10557 | — |
| 반응물 | 4-Amino-2,3,5-trimethylphenol | HCID 11105537 | — |
| 생성물 | 5-Amino-2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran hydrochloride | HCID 10220422 | 14.4% |
반응 단계
4-Amino-2,3,5-trimethylphenol (2.0 g, 13.2 mmol) and 2-methyl-2-propenol (1.15 g, 15.8 g) were heated under reflux in dichloromethane (20 ml) together with sulfuric acid (2 ml) for 18 hours. The reaction mixture was washed with aqueous saturated sodium bicarbonate solution, dried and then concentrated. The residue was purified by silica gel column chromatography (isopropyl ether). The purified product was converted into its hydrochloride and it was crystallized from ethanol-isopropyl ether to obtain the desired compound (460 mg, yield: 14.4%), m.p. 248°-250° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05594154 |
| 출처 데이터셋 | uspto-grants-1997_01 |
| ORD ID | ord-9c85de5899764bb1962a3d0000aeae6c |
| 출처 메모 | uspto-grants-1997_01 |