Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfate → 3-Methoxy-2-phenylacrylonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3-Hydroxy-2-phenylacrylonitrile | HCID 90759 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Methoxy-2-phenylacrylonitrile | HCID 54570349 | — |
반응 단계
3-Hydroxy-2-phenylacrylonitrile (12.3 g, 84.7 mmol) was dissolved in dry THF (100 ml) in a reaction vessel, and then NaH (4.1 g, 169.4 mmol) was slowly added thereto. The mixture was stirred at room temperature for 2 hr. Thereafter, dimethyl sulfate (13.7 ml, 144.0 mmol) was added, followed by stirring at 40° C. for 12 hr. After completion of the reaction, the reaction mixture was washed with distilled water and concentrated under reduced pressure. The concentrate was diluted with EtOAc and extracted with EtOAc together with distilled water. The organic layer was dried over anhydrous MgSO4 and filtered. The filtrate was concentrated under reduced pressure to give 17.9 g (112.5 mmol, quant.) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09260448B2 |
| 출처 데이터셋 | uspto-grants-2016_02 |
| ORD ID | ord-4e918329aedb4a6db664e41000b0f177 |
| 출처 메모 | uspto-grants-2016_02 |