참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butyl mercaptan | HCID 6387 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-benzyl-6-chloro-1-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione | HCID 19811548 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 178454938 | HCID 178454938 | 54% |
반응 단계
A mixture of 3-benzyl-6-chloro-1-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione (0.5 g), tert-butylmercaptan (0.1 ml) and potassium carbonate (0.14 g) in acetonitrile (10 ml) was heated under reflux for 8 hours with stirring. The reaction mixture was allowed to cool and the precipitate was removed by filtration. The filtrate was concentrated to dryness. The resulting residue was dissolved in methanol (15 ml) and 1N hydrochloric acid (1 ml) and the mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated to dryness and then the residue was extracted with methylene chloride-water. The organic layer was washed with water, dried, and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel to give pale yellow amorphous powders (0.2 g, 54%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05162326 |
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| 출처 데이터셋 | uspto-grants-1992_11 |
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| ORD ID | ord-94cddd58c3994aea8533f2a428d56d77 |
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| 출처 메모 | uspto-grants-1992_11 |
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