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1.
The cycloaddition of α,β-epoxyaldehydes or ketones () with the ketene acetal MeHC=C(OMe)2 () gives epoxyoxetanes () in high yields. Without isolation they can be transformed into 4-hydroxy-5-(1-hydroxyalkyl)-γ-butyrolactones () via the epoxy esters and trihydroxy esters (). The lactones appear to be valuable precursors for the synthesis of 5-(1-hydroxyalkyl)-3-methyl-2-5H-furanones () and 3-methyl-5-ylidene-2-5H-furanones () 相似文献
2.
The N-hydroxyazetidines and are prepared startinfrom 2,3-dihydroazete 1-oxides ( and 0 by reduction with sodium borohydride and by reaction with a nucleophile, respectively. The N-thydroxyazetidines and can be oxidized with mercury (II) oxide to the corresponding nitrones ; oxidation of the N-hydroxyazetidine (unsubstituted at C-4) with equivalent of lead tetraacetate tyields the N-tacetoxy β-lactam . 相似文献
3.
A synthesis of (2S,3S,7S)-3,7-dimethylpentadecan-2-yl acetate () and propionate () is described. (2S)-2-Methyldecan-1-yl lithium () was reacted with (3S,4S)-3,4-dimethyl-γ-butyrolactone () to yield the ketoalcohol which upon Huang-Minlon reduction furnished (2S,3S,7S)-3,7-dimethylpentadecan-2-ol (). Acylations gave the esters and . The (2S)-2-methyldecan-1-yl lithium was obtained via asymmetric synthesis. The chiral lactone was obtained from (2S,3S)-trans-2,3-epoxybutane and dimethyl malonate. 相似文献
4.
tert-Butyl azidoformate () reacts with the conjugate bases of , , (R1 = R2 = CH3), and (R1 = CH3, R2 = H) to give products [, , , and , respectively] in addition to the expected N-(tert-butoxycarbonyl)indole derivatives. 相似文献
5.
Tatsuhiko Kanmera Sannamu Lee Haruhiko Aoyagi Nobuo Izumiya 《Tetrahedron letters》1979,20(46):4483-4486
A series of cyclo (Δaminoacyl-L-Ala) () (Δ=α,β-dehydro) were prepared from cyclo(Gly-L-Ala) and corresponding aldehyde, and hydrogenated with Pd black in MeOH. Chiral inductions producing cyclo (L-aminoacyl-L-Ala) () from were 96–99% in the case of L-Aba (2-aminobutanoic acid), L-Val, L-Leu, and L-App (2-amino-5-phenylpentanoic acid) as an L-aminoacyl moiety in . Pure L-Leu, L-Aba, and L-App were synthesized in preparative scale from corresponding through asymmetric hydrogenation and acid-hydrolysis. 相似文献
6.
7.
《Tetrahedron》1987,43(13):3021-3030
A new synthesis of 9,10-dimethoxy-1,3,4,6,7,11b-hexahydro-2H-benzo aquinolizin-2-one ( and its 3-ethyl derivative via the corresponding 2-(3,4-dimethoxyphenyl)-4-piperidone ethylene acetals is reported. Alkylation of 2-arylpipendires with 2-bromoethanol followed by oxidation of the resulting amino alcohols with oxalyl chloride and dimethyl sulfoxide afforded the aldehydes , which were cyclized with hydrochloric acid to give 7-hydroxybenzo[α]quinolizidines . The reduction of with trinethylsilane and subsequent acid hydrolysis led to benzo aquinolizidin-2-ones . 相似文献
8.
Toshiyuki Yamashita Takeo Fujino Norio Masaki Hiroaki Tagawa 《Journal of solid state chemistry》1981,37(2):133-139
The structural parameters of α- and β-CdUO4 crystals are determined by X-ray powder diffraction technique. α-CdUO4 is rhombohedral and cell parameters are a = 6.233(3) Å and α = 36.12(5)°. β-CdUO4 crystallizes in a C-centered orthorhombic cell with a = 7.023(4), b = 6.849(3), c = 3.514 (2) Å. The space groups are for α-CdUO4 and Cmmm for β-CdUO4. α-CdUO4: 1U in (000), 1Cd in (), 2O(1) in ±(uuu), 2O(2) in ±(vvv); u = 0.113, v = 0.350, Z = 1. β-CdUO4: 2U in (), 2Cd in (), 4O(1) in (), 4O(2) in (); x = 0.159, y = 0.278, Z = 2. β-CdUO4 contains collinear uranyl UO2+2 groups with a UO(1) distance of 1.91 Å, located either along or parallel to the c axis whereas the UO(1) bond length in α-CdUO4 is 1.98 Å which is longer than the usual uranyl bond length. 相似文献
9.
10.
Masamichi Maruta Satoshi Kubota Narihiko Yoshimura Tomoya Kitazume Nobuo Ishikawa 《Journal of fluorine chemistry》1980,16(1):75-88
4-Fluoro-2-(-ethyl)-3-(-methyl)-1, 5-benzoxazepine was prepared by reaction of -2-methyl-2-pentene with 2-aminophenol in the presence of triethylamine in diethyl ether. The reaction of -2,4-dimethyl-3-heptene with 2-aminophenol in dimethylformamide gave 7-(-1-methylethyl)-8- (-ethyl)-9,14-benzoxazepino[4,3-b]1,6-benzoxazepine. Several ortho-bifunctional benzenes reacted similarly with -2-methyl-2-pentene and -2,4-dimethyl-3-heptene to give the corresponding seven-membered benzoheterocycles. 相似文献
11.
E.G. Frandsen 《Tetrahedron》1977,33(8):869-873
The reaction of 4- and 5-aryl-3-methylthio-1,2-dithiolylium iodides with 4-hydroxy-6-methyl-2-pyran-2-one and 4-hydroxycoumarin has been studied. 4-Substituted salts yielded 3-aryl-7-methyl-2-thioxo-2,5-pyrano [3,2-c]pyran-5-ones and 3-aryl-2-thioxo-2H,5H-pyrano[3,2-c]benzo[e]pyran-5-ones, respectively, whereas 5-substituted salts gave rise to 3-(5′-aryl-1′,2′-dithiol-3′-ylidene)-6-methyl-2-pyran-2,4-diones and 3-(5′-aryl-1′,2′-dithiol-3′-ylidene)-2-benzo [b]-pyran-2,4-diones. 相似文献
12.
Wolfgang Oppolzer Mark Kurth Daniel Reichlin Frank Moffatt 《Tetrahedron letters》1981,22(27):2545-2548
The chiral induction in the Diels-Alder addition → , assessed reliably by 19F-NMR-spectroscopy of the endo-esters , varied between 47 - 93% in favor of the 2-(R)-adducts depending on the auxiliary chiral group and the Lewis-acid catalyst. 相似文献
13.
trans- -Isopropenyl-4-methylene-spiro[2.x]alkanes ( and ) react at 0°C with CSI to give as major products the trans bicyclic cycloazanondienones (-) and as the minor products bicyclodihydro-azepinones ( and ), and the respective cis isomer of bicyclic cycloazanondienones ( and ). 相似文献
14.
Ronald D. Brown Peter D. Godfrey Donald C. McGilvery Jonathan G. Crofts 《Chemical physics letters》1981,84(3):437-439
Microwave—optical double resonance signals have been detected in a mass-selected ion-beam spectrometer for 12C16O+. With the optical excitation of fluorescence from the R1 () line of the (0,0) band of the A2Π ← X2∑ transition of 20350.6 cm?1, the microwave resonances occurred at 118101.8 ± 0.2 MHz and at 117694 ± 2 MHz corresponding to the N= 1, J = ← N = 0, J = and the N = 1, J = ← N = 0, J = transitions. 相似文献
15.
1-Methyl-2-(1′-cyano-1′-trimethylsilyloxy)alkyl-1H-imidazoles () were easily prepared from the corresponding stable carbonyl compounds, 1-methyl-2-acyl- 1H-imidazoles (). When the quarternary salts of were treated with various nucleophiles, reactive acyl species, which was presumed to be acylcyanide (), was generated in situ under CC bond fission to result in producing the corresponding acylated compounds (–) in good yields. 相似文献
16.
Bis(N-(1-benzoyl-2-propylidene)-2-pyridylmethylaminato)iron(III) hexafluorophosphate (Fe(bzpa)2PF6 is shown to be a spin-equilibrium compound between low- (S = ) and high- (S = ) spin states depending on temperature, and to have the unusual property that the relaxation time of the spin change is shorter than the Mössbauer lifetime (1 × 10?7s) of iron- 57 (l = ) in the solid state. 相似文献
17.
Photochemical cycloaddition of cyclopentene with enone esters containing different chiral auxiliaries yielded anti and syn adducts and in good yield and with moderate to high (79%) enantiomeric excesses. 相似文献
18.
A tritriacontanucleotide which has the sequence of the 5half molecule of E.coli glycine tRNA2, was synthesized by the phosphotriester method involving p-anisidate protection for the 3phosphate ends. Di- and trinucleotide units were prepared from 5dimethoxytrityl-2O-tetrahydrofuranyl-3?-O-(o-chlorophenyl)phosphoryl derivatives of uridine, N-benzoylcytidine, N-benzolyadenosine and N-iso-butyrylguanosine by condensation with 35unprotected nucleosides followed by phosphorylation to give 3phosphodiester blocks. The 3terminal dimers and trimers were synthesized by using 3(o- chlorophenyl)phosphoro-p-anisidates instead of 3?,5?-unprotected nucleosides. The 3?-phosphodiesters of oligonucleotides with a chain length of larger than 5 were obtained by removal of the 3?-phosphoro-p-anisidate with isoamyl nitrite. The 5dimethoxytrityl group was removed by treatment with zinc bromide under anhydrous conditions. Fragments were designed to use common dimer blocks and to reduce the step for 5deblocking of larger fragments. Finally a 3phosphodiester block with a chain length of 20 was condensed with a 5OH component (tridecanucleotide). The fully protected 33 mer was deblocked and purified by chromatography. The structural integrity of the product was confirmed by mobility shift analysis and complete digestion with RNase T2. 相似文献
19.
4-O-(2,6-diamino-2,3,4,6-tetradeoxy-3-C-methyl-β-L-arabino and lyxo-hexopyranosyl) and 4-O-(2-amino2,3,4,6-tetradeoxy-5-c-methyl-L-threo-hexopyranosyl-6-O-(3-amino-3-decxy-α-D-glucopyranosyl)-2-deoxystreptamine (, and ) were synthesized from a kanamycin B derivative () by regiospecific methylation and stereospecific hydrogenation followed by removal of masking groups, converting a D-sugar moiety (4-O-glycoside portion) into L-sugar. The usual conformation of and were determined as boat and skew by 250 MHz PMR spectra respectively. 相似文献
20.
Titanium(IV) chloride-mediated reaction of 4,5-dihydro-2-(trimethylsiloxy)-3-(trimethylsilyl)furan (1a) with acetaldehyde gave (3S*, 1′R*)-4,5-dihydro-3-(1′hydroxyethyl)-3-(trimethylsilyl)-2(3)furanone (2a), which afforded selectively either (Z)- or (E)-α-ethylidene-γ-butyrolactone (3a) under proper conditions. Facile isomerization of 2a into (3S*, 1′R*)-4,5-dihydro-3-&{1′-(trimethylsiloxy)ethyl}-2(3)furanone (4) suggests an intriguing stereochemical outcome from 2a to (E)-3a via an enolate of 4. 相似文献