Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
18-Crown-6 → 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 18-Crown-6 | HCID 28557 | — |
| 반응물 | 3-Chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927406 | — |
| 반응물 | Potassium phenoxide | HCID 23670670 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide | HCID 19927487 | — |
반응 단계
A mixture of 1.4 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.63 g of potassium phenolate is heated at reflux temperature in the presence of a spatula tip of 18-crown-6 in 15 ml of acetonitrile. After 19 hours, the reaction mixture is filtered through Celite® and concentrated by evaporation, and the crude product is purified by column chromatography (eluant 25% ethyl acetate/n-hexane) to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide in the form of white crystals, m.p. 155°-157° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05428002 |
| 출처 데이터셋 | uspto-grants-1995_06 |
| ORD ID | ord-85c2ecd43fd34e1c8da55ae9f327b579 |
| 출처 메모 | uspto-grants-1995_06 |