Synthesis of (5R*,6R*,7S*)-6-iodo-1,5,6,7-tetrahydro-4,1-benzoxazonin-3(2H)-ones

New 6-iodo-1,5,6,7-tetrahydro-3H-4,1-benzoxazonin-3-ones have been synthesized by reaction of N-tosyl- and N-(2-nitrobenzenesulfonyl)-N-[2-(alkenyl)phenyl]aminoacetic acids with molecular iodine.     

Combinatorial solution-phase synthesis of alkyl (1S*,2S*,3R*,5R*,6R*)-1-alkyl-3-aryl-6-benzoylamino-1-hydroxy-7- oxo-5-phenylhexahydropyrazolo[1,2-a]pyrazole-2-carboxylates

Combinatorial solution-phase cycloadditions of (1Z,4R*,5R*)-4-benzoylamino-5-phenylpyrazolidin-3-on-1-azomethine imines 3 to beta-keto esters 4 afforded a library of 26 bicyclic pyrazolidinones 5 in 6-89% yields and in 14-100% de. All products were isolated in >90% purity according to 1H NMR, and 25 of them were analytically pure. The structures of cycloadducts were confirmed by NMR and X-ray diffraction. Most of the products were isolated as mixtures of the major (1S*,2S*,3R*,5R*,6R*)-epimers 5 and the minor (1R*,2S*,3R*,5R*,6R*)-epimers 6. Epimerization of cycloadducts 5/6 at the anomeric position 1 in solution was confirmed by 1H NMR.     

Crystal Structures of rac-Methyl- (3R*, 3aS*, 4R*, 7R*, 7aR*)-7-Acetoxymethyl)-3-benzyl-4,5-dimethyl-1-oxo-3a,4,7,7a-tetrahydroisoindoline-7a-carboxylate

The X-ray structures of the compounds 4 and 2 have been determined by direct methods and refined by least squares techniques. Crystals of C₂₂H₂₇NO₅ and C₂₇H₂₇NO₅ are triclinic, space groups Pī with lattice parameters a = 13.652 (5) Å, b = 10.926 (3) Å, c = 7.755 (2) Å, a = 111.554 (4) Å, β = 85.541 (3) Å, γ = 104.813 (4) Å, and a = 15.394 (4) Å, b = 9.674 (3) Å, c = 8.522 (3) Å, a = 111.04 (4) Å, ß = 93.65 (4) Å, γ = 95.01 (4) Å, respectively.     

(5R*, 9S*)- and (5R*, 9R*)-2,2,9-Trimethyl-1,6-dioxaspiro[4.4]non-3-ene and their Dihydro Derivatives as New Constituents of Geranium Oil

(5 R^*,9S^*)- and (5R^*,9R^*)-2,2,9-Trimethyl-1,6-dioxaspiro [4.4]non-3-ene ( 1a and 1b resp.) and their dihydro derivatives 2a and 2b are described as new constituents of geranium oil. The structures and configurations of 1a , 1b , 2a , and 2b , are based on spectra interpretation and syntheses. Also some other monoterpenoid constituents identified in the same boiling range are discussed.