Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Bicarbonate → 1-{[3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 5-Ethyl-6-phenylthio-2,4-pyrimidinedione | HCID 10586637 | — |
| 반응물 | [3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl bromide | HCID 54350482 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-{[3,4-Di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedione | HCID 69976644 | — |
반응 단계
A mixture of 5-ethyl-6-phenylthio-2,4-pyrimidinedione (0.16 g, 0.66 mmol) and [3,4-di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl bromide (0.30 g, 0.66 mmol) in dimethylformamide (10 ml) were heated at 50° C. for overnight in the presence of sodium bicarbonate (66 mg, 0.79 mmol). After the concentration of dimethylformamide, 1-{[3,4-di(t-butyldimethylsilyloxymethyl)cyclopent-1-en-1-yl]methyl}-5-ethyl-6-phenylthio-2,4-pyrimidinedione was obtained by the separation of the column chromatography. And then, this compound in THF (10 ml) was reacted with n-tetrabutylammonium fluoride at room temperature for 1 hr. After the concentration of THF, the residue was separated by column chromatography to give a desirable product (48 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05922727 |
| 출처 데이터셋 | uspto-grants-1999_07 |
| ORD ID | ord-6f843d2e17714f198a85b4db06a30bbc |
| 출처 메모 | uspto-grants-1999_07 |