참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Acetyl chloride | HCID 6367 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide | HCID 19927417 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Acetoxy-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927387 | — |
반응 단계
1.3 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) are dissolved in 10 ml of tetrahydrofuran, and 0.6 ml of triethylamine is added to the solution which is then treated dropwise at 25° C. (internal temperature) with 0.5 ml of acetyl chloride. After subsequently stirring for 2 hours at room temperature, the reaction mixture is treated with ice-water and dilute hydrochloric acid and extracted with ethyl acetate, and the organic phase is washed with sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. Column chromatography on silica gel [eluant: ethyl acetate/n-hexane (2:3)] yields 3-acetoxy-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide in the form of white crystals, m.p. 119°-120° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05428002 |
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| 출처 데이터셋 | uspto-grants-1995_06 |
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| ORD ID | ord-6e8bbe39c65b4649a8217bfb868323d0 |
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| 출처 메모 | uspto-grants-1995_06 |
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