참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methanethioamide | HCID 3005587 | — |
| 반응물 | 3-Chloro-1-ethoxycarbonylpiperidin-4-one | HCID 13226155 | — |
| 생성물 | 6-Ethoxycarbonyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridine | HCID 22563507 | — |
반응 단계
To the thioformamide this obtained was added 3-chloro-1-ethoxycarbonylpiperidin-4-one (5.141 g, 25 mmole) in ethanol (100 ml) prepared according to the method described in Tetrahedron, 39, 3767 (1983) and heated at reflux in the presence of Molecular Sieves 4A for 15 hours. The reaction mixture was cooled to room temperature. After a saturated aqueous sodium hydrogen carbonate solution was added to the mixture under ice-cooling, ethanol was evaporated under reduced pressure. The reaction mixture was extracted with chloroform, washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give 6.175 g of a crude product. The product was purified by column chromatography on silica gel (C-200=150 g, eluent:CHCl3) to give 3.213 g of the title compound as a clear pale yellow oily product (yield, 60.5%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05594004 |
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| 출처 데이터셋 | uspto-grants-1997_01 |
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| ORD ID | ord-4dc0cb30e2c94e49ac651c95172a31d7 |
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| 출처 메모 | uspto-grants-1997_01 |
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