Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetonitrile → acrylic acid 4-{2-hydroxy-3-[2-(9-oxo-9H-thioxanthen-2-yloxy)-acetoxy]-propoxy}-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 2-(Carboxymethoxy)thioxanthone | HCID 3019853 | — |
| 반응물 | 4-Hydroxybutylacrylate glycidylether | HCID 22323150 | — |
| 촉매 | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | acrylic acid 4-{2-hydroxy-3-[2-(9-oxo-9H-thioxanthen-2-yloxy)-acetoxy]-propoxy}-butyl ester | HCID 58325515 | 144.2% |
반응 단계
A reaction mixture containing (9-oxo-9H-thioxanthen-2-yloxy)acetic acid (4.0 g, 14 mmol), acetonitrile (55 ml), dimethylacetamide (10 mL), tetrabutylammonium bromide (0.5 g, 1.4 mmol) and 2,6-di-tert-butyl-4-methylphenol (0.03 g, 0.114 mmol) was heated to reflux. At this temperature 4-hydroxybutylacrylate glycidylether (2.3 g, 11.4 mmol) was added and the mixture was allowed to stir at reflux temperature for 16 hours. The mixture was cooled to room temperature and the solvent was evaporated under reduced pressure to provide 8.0 g of a yellow oil. The product was purified on a Prochrom LC80 Column using dichloromethane/ethyl acetate (60/40) as eluent on Kromasil Si60A 10 μm, to afford 1.8 g of a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08530510B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-acc68d80e21b4ef89d1abdc17d452554 |
| 출처 메모 | uspto-grants-2013_09 |