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【结 构 式】 
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【分子编号】31191 【品名】S-(2-chloro-1-methyl-2-oxoethyl) 2-thiophenecarbothioate 【CA登记号】 |
【 分 子 式 】C8H7ClO2S2 【 分 子 量 】234.72708 【元素组成】C 40.94% H 3.01% Cl 15.1% O 13.63% S 27.32% |
合成路线1
该中间体在本合成路线中的序号：(IV)Triethylamine is added to thiolactic acid (I) and 2-thiophencarbonyl chloride (II) in tetrahydrofuran. Mix is cooled at -5 C under agitation and thionyl chloride is added keeping the temperature between 0 and 10 C. A solution of homocysteine thiolactone hydrochloride and triethylamine in water is then added to the reaction, keeping the temperature below 10 C. The reaction is carried out for 1 h at room temperature under agitation, after which the solvent is evaporated at reduced pressure. Water is used to wash and diethyl ether to extract. The organic phase is dried on Na2SO4 anhydrous and the solvent is eliminated at reduced pressure. The raw product obtained from a mix of dichloromethane/diethyl ether (60/40) is crystallized (MR-889).
| 【1】 Quadro, G.; MR-889. Drugs Fut 1990, 15, 10, 997. |
| 中间体序号 | 中间体编号 | 品名 | CAS号 | 分子式 | 供应商 | 用于合成 |
|---|---|---|---|---|---|---|
| (I) | 24361 | 2-sulfanylpropionic acid; 2-mercaptopropionic acid | 57965-30-7 | C3H6O2S | 详情 | 详情 |
| (II) | 14103 | 2-Thiophenecarbonyl chloride | 5271-67-0 | C5H3ClOS | 详情 | 详情 |
| (III) | 31190 | 2-[(2-thienylcarbonyl)sulfanyl]propionic acid | C8H8O3S2 | 详情 | 详情 | |
| (IV) | 31191 | S-(2-chloro-1-methyl-2-oxoethyl) 2-thiophenecarbothioate | C8H7ClO2S2 | 详情 | 详情 | |
| (V) | 22495 | 3-aminodihydro-2(3H)-thiophenone | 10593-85-8 | C4H7NOS | 详情 | 详情 |