Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,2-Difluoropropane-1,3-diol → 1,3-Dioxane, 5,5-difluoro-2-[(phenylmethoxy)methyl]-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,2-Difluoropropane-1,3-diol | HCID 95744 | — |
| 반응물 | (Phenylmethoxy)acetaldehyde | HCID 108989 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1,3-Dioxane, 5,5-difluoro-2-[(phenylmethoxy)methyl]- | HCID 59792487 | 42.8% |
반응 단계
A mixture of 2,2-difluoropropane-1,3-diol (1 g, 8.9 mmol), benzyloxyacetaldehyde (1.34 g, 8.9 mmol), p-toluenesulfonic acid monohydrate (154 mg, 0.81 mmol) and toluene (20 ml) was heated under reflux by a condenser equipped with a Dean-Stark apparatus for one hour. The resultant mixture was stirred at room temperature overnight and then the reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate and silica gel was added thereto. The resultant mixture was concentrated to dryness and subjected to silica gel column chromatography (elution solvent: n-heptane/ethyl acetate=10/1) to obtain the title compound (930 mg, 42.8%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425634B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-97711e84e9294c079076706531e3404f |
| 출처 메모 | uspto-grants-2008_09 |