Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 2,3-Dihydrobenzofuran-5-carboxaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Dihydrobenzofuran | HCID 10329 | — |
| 반응물 | Methane, dichloromethoxy- | HCID 21004 | — |
| 촉매 | Diamminetetrachlorotitanate(IV) | HCID 160960 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2,3-Dihydrobenzofuran-5-carboxaldehyde | HCID 735901 | 61,555.602% |
반응 단계
Titanium chloride (28 ml) was dropwise added to a dichloromethane (100 ml) solution containing 2,3-dihydrobenzofuran (10.0 g, 83.2 mmols) and dichloromethyl methyl ether (11.3 ml, 0.125 mmols), while cooling with ice. The mixture was stirred for 1 hour, while still cooling with ice, and then water was added thereto. Dichloromethane was removed under reduced pressure, and the residue was extracted with ethyl acetate. The extract was washed with a saturated saline solution, then dried with anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified through silica-gel chromatography (hexane/ethyl acetate=1/1) to obtain 11.4 g (yield: 92%) of the target compound. This was oily.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06218429B1 |
| 출처 데이터셋 | uspto-grants-2001_04 |
| ORD ID | ord-e60d3f4560d94190a849d10d23a90938 |
| 출처 메모 | uspto-grants-2001_04 |