Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-Methyl-5-(2-methyl-1,3-dioxolan-2-yl)aniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 3'-Nitro-4'-methylacetophenone | HCID 79246 | — |
| 용매 | Ethylene Glycol | HCID 174 | — |
| 생성물 | 2-Methyl-5-(2-methyl-1,3-dioxolan-2-yl)aniline | HCID 66882066 | 94% |
반응 단계
To a flask mounted with Dean-Stark water removing apparatus (Dean-Stark trap) were added toluene (200 ml), 4-methyl-3-nitroacetophenone (9.77 g, 54.53 mmol), ethylene glycol (4.6 ml) and p-toluenesulfonic acid.monohydrate (0.79 g), and the mixture was heated under reflux for 100 min. The reaction mixture was cooled, washed with diluted aqueous sodium hydroxide solution and saturated brine, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give a crude brown oil (13.0 g). Using the crude oil and according to the method of Reference Example 61, step B, the title compound (9.89 g, yield 94%) was obtained as a pale-yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08513235B2 |
| 출처 데이터셋 | uspto-grants-2013_08 |
| ORD ID | ord-9798094bdea14ce180d24232641e453d |
| 출처 메모 | uspto-grants-2013_08 |