Enantioselective sequential Michael addition/C-H olefination/Michael reaction for the efficient collective synthesis of clavine alkaloids
Source abstract
Abstract
Sequential reactions are important for the direct and convenient synthesis of complex molecules with multiple chiral centers. Here, we report an enantioselective sequential Michael addition/C–H olefination/Michael addition reaction for the asymmetric construction of chiral 2-aminotetralin derivatives bearing three stereogenic centers using readily accessible 2-aryl N-quinolyl acrylamide, nitromethane, and alkenyl iodide. This optimized process utilizes a quinine-based squaramide bifunctional organocatalyst in the enantioselective Michael addition of nitromethane to a conjugated amide. Subsequently, the N,N-bidentate amide-directed Pd-catalyzed C–H olefination of the 2-arylamide and intramolecular Michael addition of a conjugated ester generates tetralins with high enantioselectivities and good stereoselectivities and yields. To demonstrate the synthetic utility of this sequential reaction, the collective synthesis of various clavine alkaloids with different skeletons is accomplished from a common tricyclic intermediate that can be readily prepared using chiral 2-aminotetralins.
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Research context
OpenAlex topics: Advanced Synthetic Organic Chemistry · Asymmetric Synthesis and Catalysis · Asymmetric Hydrogenation and Catalysis
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (50)
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1. Chapter one - biosynthesis, total synthesis, and biological profiles of Ergot alkaloids
2. Morphine, the Proteus of organic molecules10.1039/b111551k ↗
3. The quest for a practical synthesis of morphine alkaloids and their derivatives by chemoenzymatic methods10.1021/ar500427k ↗
4. Total synthesis of the Daphniphyllum alkaloid daphenylline10.1038/nchem.1694 ↗
5. Total synthesis of Longeracinphyllin A10.1021/jacs.7b09186 ↗
6. Total syntheses of Daphenylline, Daphnipaxianine A, and Himalenine D10.1002/anie.201711482 ↗
7. Concise enantioselective total synthesis of Daphenylline enabled by an intramolecular oxidative dearomatization10.1021/jacs.2c01674 ↗
8. C-9 and N-substituted analogs of cis-(3aR)-(-)-2,3,3a,4,5,9b-hexahydro-3-propyl-1H-benz[e]indole-9-carboxamide: 5-HT1A receptor agonists with various degrees of metabolic stability10.1021/jm00004a018 ↗
9. Dopamine D1/D5 receptor antagonists with improved pharmacokinetics: design, synthesis, and biological evaluation of phenol bioisosteric analogues of benzazepine D1/D5 antagonists10.1021/jm030614p ↗
10. Functional primary amines and diamines from α-aminoacids. A concise route to substituted 2-aminotetralins10.1021/ol901263t ↗
11. Stereoselective Dynamic Cyclization of Allylic Azides: Synthesis of Tetralins, Chromanes, and Tetrahydroquinolines10.1021/jacs.7b11299 ↗
12. Asymmetric organocatalytic domino reactions10.1002/anie.200603129 ↗
13. Organocatalytic cascade reactions as a new tool in total synthesis10.1038/nchem.539 ↗
14. Cascade polycyclizations in natural product synthesis10.1039/C5CS00105F ↗
15. Recent developments in natural product synthesis using metal-catalysed C–H bond functionalisation10.1039/c1cs15013h ↗
16. Multiple catalytic C−H bond functionalization for natural product synthesis10.1002/anie.202001224 ↗
17. Recent applications of C–H functionalization in complex natural product synthesis10.1039/C8CS00716K ↗
18. C–H functionalization logic in total synthesis10.1039/c0cs00182a ↗
19. Palladium-catalyzed direct intermolecular amination of unactivated methylene C(sp3)–H bonds with azodiformates via bidentate-chelation assistance10.1021/acscatal.6b03621 ↗
20. Bioinspired palladium-catalyzed intramolecular C(sp3)−H activation for the collective synthesis of proline natural products10.1002/anie.202207088 ↗
21. Lewis acid enabled copper-catalyzed asymmetric synthesis of chiral β-substituted amides10.1021/jacs.7b07344 ↗
22. Catalytic direct-type 1,4-addition reactions of alkylazaarenes10.1002/anie.201611374 ↗
23. Stereodivergent synthesis through catalytic asymmetric reversed hydroboration10.1021/jacs.8b13520 ↗
24. Copper(I)-catalyzed asymmetric 1,4-conjugate hydrophosphination of α,β-unsaturated Amides10.1021/jacs.0c09654 ↗
25. Enantioselective synthesis of tertiary boronic esters through catalytic asymmetric reversed hydroboration10.1038/s41467-021-24012-z ↗
26. Bifunctional iminophosphorane-catalyzed enantioselective sulfa-Michael addition to unactivated α,β-unsaturated amides10.1021/jacs.1c11898 ↗
27. An unexpected directing Effect in the Asymmetric Transfer Hydrogenation of α,α-Disubstituted Ketones10.1021/ol201643v ↗
28. Direct Remote Asymmetric Bisvinylogous 1,4-Additions of Cyclic 2,5-Dienones to Nitroalkenes10.1021/ol500700d ↗
29. Ergot alkaloids: structure diversity, biosynthetic gene clusters and functional proof of biosynthetic genes10.1039/C0NP00060D ↗
30. Strategies for the Total Synthesis of Clavicipitic Acid10.1002/chem.201505014 ↗
31. Total synthesis, biosynthesis and biological profiles of clavine alkaloids10.1039/C6OB00878J ↗
32. Ergot alkaloids: synthetic approaches to lysergic acid and clavine alkaloids10.1039/C6NP00110F ↗
33. Total Synthesis of Lysergic Acid10.1021/ol4019562 ↗
34. Asymmetric formal synthesis of (+)-cycloclavine10.1039/C7CC08044A ↗
35. Catalytic asymmetric formal total syntheses of (+)- and (−)-cycloclavine10.1039/C7CC09045E ↗
36. Total synthesis of (+)-Lysergic acid10.1021/jo4018777 ↗
37. Catalytic asymmetric reactions of 4-substituted indoles with nitroethene: A direct entry to ergot alkaloid structures10.1002/chem.201502655 ↗
38. Total syntheses of Pyroclavine, Festuclavine, Lysergol, and Isolysergol via a catalytic asymmetric nitro-Michael reaction10.1002/chem.201702459 ↗
39. Biomimetic Total Syntheses of Clavine Alkaloids10.1021/acs.orglett.7b03683 ↗
40. Intramolecular dearomatizing [3 + 2] annulation of α-Imino carbenoids with aryl rings furnishing 3,4-fused indole skeletons10.1021/ja412663a ↗
41. Total synthesis of (−)-Chanoclavine I and an oxygen-substituted ergoline derivative10.1021/acs.joc.7b00573 ↗
42. Synthesis of (+)-Lysergol and its analogues to assess serotonin receptor activity10.1021/acs.orglett.6b03779 ↗
43. Concise synthesis of (−)-Cycloclavine and (−)-5-epi-Cycloclavine via asymmetric C–C activation10.1021/jacs.8b05549 ↗
44. Eight-step enantioselective total synthesis of (−)-Cycloclavine10.1002/anie.201608820 ↗
45. Total syntheses of Festuclavine, Pyroclavine, Costaclavine, epi-Costaclavine, Pibocin A, 9-Deacetoxyfumigaclavine C, Fumigaclavine G, and Dihydrosetoclavine10.1021/acs.orglett.7b01504 ↗
46. Total syntheses of (−)-Hibiscone C and Lysergine: a cyclization/fragmentation strategy10.1021/acs.orglett.6b03778 ↗
47. Regioselective Direct C-4 Functionalization of Indole: Total Syntheses of (-)-Agroclavine and (-)-Elymoclavine10.1021/acs.orglett.7b01681 ↗
48. Biomimetic total syntheses of ergot alkaloids via decarboxylative Giese coupling10.1021/acs.orglett.0c03867 ↗
49. Selective removal of aminoquinoline auxiliary by IBX oxidation10.1021/acs.joc.9b01362 ↗
50. Electrophilic aromatic substitution with N-methoxy-N-acylnitrenium ions generated from N-chloro-N-methoxy amides: syntheses of nitrogen heterocyclic compounds bearing a N-methoxy amide group10.1021/jo00275a027 ↗