Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 4-(3,4-Dichlorobenzyloxy)-3-methylbenzaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 3,4-Dichlorobenzyl alcohol | HCID 15728 | — |
| 반응물 | 4-Hydroxy-3-methylbenzaldehyde | HCID 139901 | — |
| 반응물 | Diethylazodicarboxylate toluene | HCID 66777355 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(3,4-Dichlorobenzyloxy)-3-methylbenzaldehyde | HCID 23073341 | 69% |
반응 단계
4-Hydroxy-3-methylbenzaldehyde (365 mg, 2.68 mmol), 3,4-dichlorobenzyl alcohol (665 mg, 3.76 mmol), and triphenylphosphine (980 mg, 3.74 mmol) were dissolved in tetrahydrofuran (8 mL), and a diethyl azodicarboxylate toluene solution (2.2 M, 1.71 mL, 3.76 mmol) was slowly added dropwise thereto at room temperature, and then, the resulting mixture was stirred under a nitrogen atmosphere at room temperature for 2 hours. The solvent was distilled off under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 95:5 (v/v)), whereby the objective title compound was obtained as a white solid (542 mg, yield: 69%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08222281B2 |
| 출처 데이터셋 | uspto-grants-2012_07 |
| ORD ID | ord-fbada1c884f34569b25d688afebe21b2 |
| 출처 메모 | uspto-grants-2012_07 |