参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 氯甲酸氯乙酯 | HCID 12305 | — |
| 反应物 | 7-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene | HCID 131727045 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | 海萝胶 | HCID 313 | — |
| 产物 | 7-Methyl-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene | HCID 59789425 | — |
反应步骤
K2CO3 (320 mg, 2.32 mmol) was added to a solution of the product from step g) (165 mg, 0.58 mmol) in 6 mL followed by the addition of 2-chloroethylchloroformate (332 mg, 2.32 mmol) under vigorous stirring at room temperature. Next, the reaction was stirred for two hours at 75° C. after which the reaction mixture was cooled, filtered and the solvent was evaporated to leave an oily residue that was then dissolved in dry methanol (10 mL) and was stirred at room temperature for one hour. The solvent was evaporated and the residue was triturated in diethyl ether (5 mL) to give the subtitle compound as its HCl salt. MS calculated for C10H13NS+H: 180, observed: 180. 1H NMR (CDCl3300 MHz) δ 1.32 (d, 3H), 1.93 (s, 1H), 3.04 (m, 1H), 3.18 (m, 2H), 3.47 (m, 3H), 3.78 (m, 1H), 6.83 (d, 1H), 7.21 (d, 1H) ppm.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US07423056B2 |
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| 来源数据集 | uspto-grants-2008_09 |
|---|
| ORD ID | ord-85d41e6f25a74b478ea7ed29ef94133e |
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| 来源说明 | uspto-grants-2008_09 |
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