Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 7-Methyl-2,3-dihydro-1-benzofuran-3-ol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Trimethyloxosulphonium chloride | HCID 197819 | — |
| 반응물 | 3-Methylsalicylaldehyde | HCID 522777 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 7-Methyl-2,3-dihydro-1-benzofuran-3-ol | HCID 13013060 | — |
반응 단계
Under a nitrogen atmosphere 0.945 g (7.35 mmol) trimethylsulphoxonium chloride were placed in 20 mL THF, and 0.300 g (7.50 mmol) sodium hydride (55%, suspension in mineral oil) were added batchwise. The reaction mixture was refluxed for 2 h. Then 1.00 g (7.35 mmol) 2-hydroxy-3-methylbenzaldehyde in 20 mL THF were added dropwise to the reaction mixture and it was refluxed overnight. Then PE was added and the suspension obtained was filtered. The filtrate was evaporated down i. vac. and purified by flash chromatography. The fractions containing the product were combined and evaporated down.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08629137B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-83e49fa21a4c4926ac8c167607bd148d |
| 출처 메모 | uspto-grants-2014_01 |