• 文献检索
  • 文档翻译
  • 深度研究
  • 学术资讯
  • Suppr Zotero 插件Zotero 插件
  • 邀请有礼
  • 套餐&价格
  • 历史记录
应用&插件
Suppr Zotero 插件Zotero 插件浏览器插件Mac 客户端Windows 客户端微信小程序
定价
高级版会员购买积分包购买API积分包
服务
文献检索文档翻译深度研究API 文档MCP 服务
关于我们
关于 Suppr公司介绍联系我们用户协议隐私条款
关注我们

Suppr 超能文献

核心技术专利:CN118964589B侵权必究
粤ICP备2023148730 号-1Suppr @ 2026

文献检索

告别复杂PubMed语法,用中文像聊天一样搜索,搜遍4000万医学文献。AI智能推荐,让科研检索更轻松。

立即免费搜索

文件翻译

保留排版,准确专业,支持PDF/Word/PPT等文件格式,支持 12+语言互译。

免费翻译文档

深度研究

AI帮你快速写综述,25分钟生成高质量综述,智能提取关键信息,辅助科研写作。

立即免费体验

流动合成中的核磁共振反应监测

NMR reaction monitoring in flow synthesis.

作者信息

Gomez M Victoria, de la Hoz Antonio

机构信息

Área Química Orgánica, Facultad de Químicas, Universidad de Castilla-La Mancha, Avda. Camilo José Cela nº 10, E-13071 Ciudad Real, Spain and Instituto Regional de Investigación Científica Aplicada (IRICA), Avda. Camilo José Cela s/n, E-13071 Ciudad Real, Spain.

出版信息

Beilstein J Org Chem. 2017 Feb 14;13:285-300. doi: 10.3762/bjoc.13.31. eCollection 2017.

DOI:10.3762/bjoc.13.31
PMID:28326137
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5331343/
Abstract

Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed.

摘要

介绍了流动化学与核磁共振在线和联机分析联用的最新进展。综述了宏反应器和微反应器的使用,以及与包含微线圈的标准和定制核磁共振探头相结合,并集成到高分辨率和台式核磁共振仪器中的情况。收集了一些近期的特定应用,包括合成应用、动力学和热力学参数的测定以及反应优化,甚至在单实验和微升规模上也是如此。最后,讨论了允许自动反应监测和优化的软件。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/7a738bcadc33/Beilstein_J_Org_Chem-13-285-g016.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/1d39110bf65b/Beilstein_J_Org_Chem-13-285-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/21eac78c19c1/Beilstein_J_Org_Chem-13-285-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f0936fcf52ff/Beilstein_J_Org_Chem-13-285-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/313b56afa8a8/Beilstein_J_Org_Chem-13-285-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f3c599fb66ce/Beilstein_J_Org_Chem-13-285-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2fa785b361af/Beilstein_J_Org_Chem-13-285-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/402a76edf58f/Beilstein_J_Org_Chem-13-285-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/3f0db4afe7c8/Beilstein_J_Org_Chem-13-285-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/30d5f9e9bfdc/Beilstein_J_Org_Chem-13-285-g017.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/9063cd5b018b/Beilstein_J_Org_Chem-13-285-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f803e6cfd2a4/Beilstein_J_Org_Chem-13-285-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/c4acff426446/Beilstein_J_Org_Chem-13-285-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/9ec186dd0f1e/Beilstein_J_Org_Chem-13-285-g013.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2b9af552b42c/Beilstein_J_Org_Chem-13-285-g014.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2f9ba41e2e95/Beilstein_J_Org_Chem-13-285-g015.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/7a738bcadc33/Beilstein_J_Org_Chem-13-285-g016.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/1d39110bf65b/Beilstein_J_Org_Chem-13-285-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/21eac78c19c1/Beilstein_J_Org_Chem-13-285-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f0936fcf52ff/Beilstein_J_Org_Chem-13-285-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/313b56afa8a8/Beilstein_J_Org_Chem-13-285-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f3c599fb66ce/Beilstein_J_Org_Chem-13-285-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2fa785b361af/Beilstein_J_Org_Chem-13-285-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/402a76edf58f/Beilstein_J_Org_Chem-13-285-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/3f0db4afe7c8/Beilstein_J_Org_Chem-13-285-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/30d5f9e9bfdc/Beilstein_J_Org_Chem-13-285-g017.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/9063cd5b018b/Beilstein_J_Org_Chem-13-285-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/f803e6cfd2a4/Beilstein_J_Org_Chem-13-285-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/c4acff426446/Beilstein_J_Org_Chem-13-285-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/9ec186dd0f1e/Beilstein_J_Org_Chem-13-285-g013.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2b9af552b42c/Beilstein_J_Org_Chem-13-285-g014.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/2f9ba41e2e95/Beilstein_J_Org_Chem-13-285-g015.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8164/5331343/7a738bcadc33/Beilstein_J_Org_Chem-13-285-g016.jpg

相似文献

1
NMR reaction monitoring in flow synthesis.流动合成中的核磁共振反应监测
Beilstein J Org Chem. 2017 Feb 14;13:285-300. doi: 10.3762/bjoc.13.31. eCollection 2017.
2
From single to multiple microcoil flow probe NMR and related capillary techniques: a review.从单微流探针 NMR 到多微流探针 NMR 及相关毛细管技术:综述。
Anal Bioanal Chem. 2012 Jan;402(2):647-69. doi: 10.1007/s00216-011-5419-z. Epub 2011 Oct 4.
3
Utilizing on- and off-line monitoring tools to follow a kinetic resolution step during flow synthesis.
Magn Reson Chem. 2017 Apr;55(4):348-354. doi: 10.1002/mrc.4494. Epub 2016 Aug 11.
4
Reaction monitoring via benchtop nuclear magnetic resonance spectroscopy: A practical comparison of on-line stopped-flow and continuous-flow sampling methods.通过台式核磁共振光谱进行反应监测:在线停流和连续流采样方法的实际比较。
Magn Reson Chem. 2024 Apr;62(4):310-322. doi: 10.1002/mrc.5395. Epub 2023 Sep 22.
5
Integrated microreactors for reaction automation: new approaches to reaction development.集成微反应器用于反应自动化:反应开发的新方法。
Annu Rev Anal Chem (Palo Alto Calif). 2010;3:19-42. doi: 10.1146/annurev.anchem.111808.073718.
6
NMR detection with multiple solenoidal microcoils for continuous-flow capillary electrophoresis.用于连续流动毛细管电泳的多个螺线管微线圈的核磁共振检测。
Anal Chem. 2002 Nov 1;74(21):5550-5. doi: 10.1021/ac025903k.
7
Digital microfluidics and nuclear magnetic resonance spectroscopy for in situ diffusion measurements and reaction monitoring.用于原位扩散测量和反应监测的数字微流控与核磁共振光谱技术。
Lab Chip. 2019 Feb 12;19(4):641-653. doi: 10.1039/c8lc01214h.
8
Merging Gradient-Based Methods to Improve Benchtop NMR Spectroscopy: A New Tool for Flow Reaction Optimization.基于梯度的方法融合以改进台式 NMR 光谱学:用于流反应优化的新工具。
Chemphyschem. 2020 Oct 16;21(20):2311-2319. doi: 10.1002/cphc.202000573. Epub 2020 Sep 21.
9
Planar microcoil-based microfluidic NMR probes.基于平面微线圈的微流控核磁共振探头。
J Magn Reson. 2003 Oct;164(2):242-55. doi: 10.1016/s1090-7807(03)00151-4.
10
Exploration of continuous-flow benchtop NMR acquisition parameters and considerations for reaction monitoring.连续流台式 NMR 采集参数的探索及在反应监测中的考虑因素。
Magn Reson Chem. 2020 Dec;58(12):1234-1248. doi: 10.1002/mrc.5094. Epub 2020 Sep 7.

引用本文的文献

1
Boosting H and C NMR signals by orders of magnitude on a bench.在实验台上将氢和碳核磁共振信号增强几个数量级。
Sci Adv. 2024 Dec 6;10(49):eadq3780. doi: 10.1126/sciadv.adq3780. Epub 2024 Dec 4.
2
Pure Shift NMR in Continuous Flow.连续流动中的纯位移核磁共振
Chemistry. 2025 Jan 2;31(1):e202403385. doi: 10.1002/chem.202403385. Epub 2024 Nov 13.
3
Continuous flow synthesis of pyridinium salts accelerated by multi-objective Bayesian optimization with active learning.通过具有主动学习的多目标贝叶斯优化加速吡啶鎓盐的连续流动合成。

本文引用的文献

1
A self optimizing synthetic organic reactor system using real-time in-line NMR spectroscopy.一种使用实时在线核磁共振光谱法的自优化合成有机反应器系统。
Chem Sci. 2015 Feb 1;6(2):1258-1264. doi: 10.1039/c4sc03075c. Epub 2014 Nov 14.
2
Simple 3D Printed Scaffold-Removal Method for the Fabrication of Intricate Microfluidic Devices.用于制造复杂微流控器件的简单3D打印支架去除方法。
Adv Sci (Weinh). 2015 Jul 16;2(9):1500125. doi: 10.1002/advs.201500125. eCollection 2015 Sep.
3
Enabling Technologies for the Future of Chemical Synthesis.
Chem Sci. 2023 Jul 12;14(30):8061-8069. doi: 10.1039/d3sc01303k. eCollection 2023 Aug 2.
4
Multinuclear 1D and 2D NMR with F-Photo-CIDNP hyperpolarization in a microfluidic chip with untuned microcoil.微流控芯片中未调谐微线圈的多核 1D 和 2D NMR 与 F-Photo-CIDNP 超极化
Nat Commun. 2023 Jun 30;14(1):3885. doi: 10.1038/s41467-023-39537-8.
5
Online Monitoring of Small Volume Reactions Using Compact Liquid Chromatography Instrumentation.使用紧凑型液相色谱仪器对小体积反应进行在线监测。
Sep Sci Plus. 2022 Jun;5(6):213-219. doi: 10.1002/sscp.202200012. Epub 2022 Mar 31.
6
Benchtop F Nuclear Magnetic Resonance (NMR) Spectroscopy Provides Mechanistic Insight into the Biginelli Condensation toward the Chemical Synthesis of Novel Trifluorinated Dihydro- and Tetrahydropyrimidinones as Antiproliferative Agents.台式F核磁共振(NMR)光谱为新型三氟代二氢和四氢嘧啶酮作为抗增殖剂的化学合成中的Biginelli缩合反应提供了机理见解。
ACS Omega. 2023 Mar 10;8(11):10545-10554. doi: 10.1021/acsomega.3c00290. eCollection 2023 Mar 21.
7
Automated Segmented-Flow Analysis - NMR with a Novel Fluoropolymer Flow Cell for High-Throughput Screening.自动化分段流分析 - 新型氟聚合物流池的 NMR 用于高通量筛选。
Anal Chem. 2022 Nov 8;94(44):15350-15358. doi: 10.1021/acs.analchem.2c03038. Epub 2022 Oct 27.
8
RotoMate: An open-source, 3D printed autosampler for use with benchtop nuclear magnetic resonance spectrometers.RotoMate:一种用于台式核磁共振光谱仪的开源3D打印自动进样器。
HardwareX. 2021 Jun 23;10:e00211. doi: 10.1016/j.ohx.2021.e00211. eCollection 2021 Oct.
9
Chemputation and the Standardization of Chemical Informatics.化学计算与化学信息学的标准化
JACS Au. 2021 Aug 31;1(10):1572-1587. doi: 10.1021/jacsau.1c00303. eCollection 2021 Oct 25.
10
A Nuclear Magnetic Resonance (NMR) Platform for Real-Time Metabolic Monitoring of Bioprocesses.一种用于生物工艺实时代谢监测的核磁共振(NMR)平台。
Molecules. 2020 Oct 13;25(20):4675. doi: 10.3390/molecules25204675.
未来化学合成的使能技术。
ACS Cent Sci. 2016 Mar 23;2(3):131-8. doi: 10.1021/acscentsci.6b00015. Epub 2016 Feb 24.
4
On-demand continuous-flow production of pharmaceuticals in a compact, reconfigurable system.按需在紧凑、可重构系统中连续流生产药物。
Science. 2016 Apr 1;352(6281):61-7. doi: 10.1126/science.aaf1337.
5
Towards dial-a-molecule by integrating continuous flow, analytics and self-optimisation.通过整合连续流动、分析和自我优化实现按需定制分子。
Chem Soc Rev. 2016 Apr 21;45(8):2032-43. doi: 10.1039/c5cs00793c. Epub 2016 Jan 27.
6
Determination of Kinetic Parameters within a Single Nonisothermal On-Flow Experiment by Nanoliter NMR Spectroscopy.纳升级 NMR 光谱法在单次非等温流动实验中确定动力学参数。
Anal Chem. 2015 Oct 20;87(20):10547-55. doi: 10.1021/acs.analchem.5b02811. Epub 2015 Oct 2.
7
Flow "Fine" Synthesis: High Yielding and Selective Organic Synthesis by Flow Methods.流动“精细”合成:通过流动方法实现的高产率和高选择性有机合成。
Chem Asian J. 2016 Feb 18;11(4):425-36. doi: 10.1002/asia.201500916. Epub 2015 Oct 20.
8
Reaction monitoring using online vs tube NMR spectroscopy: seriously different results.使用在线核磁共振光谱与试管核磁共振光谱进行反应监测:结果差异显著。
Magn Reson Chem. 2016 Jun;54(6):451-6. doi: 10.1002/mrc.4259. Epub 2015 Aug 6.
9
Rapid-melt Dynamic Nuclear Polarization.快速熔融动态核极化。
J Magn Reson. 2015 Sep;258:40-8. doi: 10.1016/j.jmr.2015.06.007. Epub 2015 Jul 6.
10
Machine-Assisted Organic Synthesis.机器辅助有机合成
Angew Chem Int Ed Engl. 2015 Aug 24;54(35):10122-36. doi: 10.1002/anie.201501618. Epub 2015 Jul 16.