|
| Rh(I)中间体及抗高血压药物用手性催化剂的合成及性能研究 |
| Synthesis, characterization and catalytic performance of [Rh(COD)(S,S)-Meduphos)] in the antihypertensive drug Ramipril |
| Received:September 18, 2022 |
| DOI： |
| 中文关键词: 二(乙烯)氯铑二聚体 (+)-1,2-双((2S,5S)-2,5-二甲基膦基)苯(1,5-环辛二烯)四氟硼酸铑(I) 合成 结构 催化性能 |
| 英文关键词: [RhCl(C2H4)2]2 [Rh(COD)(S,S)-Meduphos)]BF4 synthesis structure catalytic activity |
| 基金项目:国家自然科学基金(52361006)；云南省转制科研院所技术开发研究专项(202104AR040016)；云南省科重大科技专项(202002AB080002、202102AB080007)；云南贵金属实验室有限公司科技计划项目(YPML-2022050231) |
| Author Name | Affiliation | | LIU Guihua | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | GUO Xuhu | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | GAO Anli | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | YANG Jun | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | FAN Xingqiang | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | XU Mingming | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China | | YU Juan | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Yunnan Precious Metals Laboratory Co. Ltd., Kunming 650106, China |
|
| Hits: 488 |
| Download times: 287 |
| 中文摘要: |
| 在微压状态下，以95%的乙醇为溶剂，三氯化铑、乙烯等为原料，合成了Rh(I)中间体，产率85%；再以该中间体、1,5-环辛二烯、四氟硼酸银和(+)-1,2-双((2S,5S)-2,5-二甲基膦基)苯为原料，四氢呋喃为溶剂合成了Rh(I)手性催化剂，产率91.09%。采用元素分析、1H-NMR、13C-NMR、MS-ESI+和IR对其化学结构进行了表征。以合成抗高血压药物雷米普利为反应模型进行催化活性评价，结果表明，该手性催化剂与商业对照品的催化活性相当，转化率≥70%，产品光学纯度≥98%。 |
| 英文摘要: |
| Under the condition of micro-pressure, the Rh(I) intermediate was prepared in one-step process from RhCl3.3H2O in 95% ethanol solvent by filling with ethylene gas. The ylied was ≥85%. A quqntitative reaction of the Rh(I) intermediate with 1,5-cyclooctandiene, AgBF4 and (S,S)-meduphos in tetrahydrofuran produced the desired chiral catalyst [Rh(COD)(S,S)-Meduphos)]BF4 with a yield of 91.09%. The structrues were confirmed by means of elemental analysis, 1H-NMR, 13C-NMR, FT-IR and MS-ESI+. The catalytic activity in the preparation of Ramipril was found to be ≥70% in terms of the conversion rate and optical purity of the product was 98% ee, comparable to the activity and selectivity obtained by using the commercially available catalyst. |
|
View Full Text
View/Add Comment Download reader |
| Close |
|
|
|