2-oxo-l-butyl

Te-NMR spectroscopic investigations ascertained the presence of the isomeric ketonyl tellurium trichlorides in the reaction mixtures. The isomers with tellurium on the less hindered carbon atom are generally the predominant species. Only 2-butanone yielded the 2-oxo-3-butyl tellurium trichloride as the major compound1, in which the tellurium is bonded to the more hindered carbon atom. Morgan2 claimed this compound to be 2-oxo-l-butyl tellurium trichloride. The symmetrical diketonyl tellurium dichlorides with tellurium bonded to the least hindered carbon were the only dichlorides detected1. 

Dimethyl-2-oxo-l-butyl 4-Methoxyphenyl Tellurium Dichloride1 A suspension of 1.02 g (3.0 mmol) of 4-methoxyphenyl tellurium trichloride in 10 m/ benzene is mixed with 0.516 g (3.0 mmol) 3,3-dimethyl-2-trimethylsiloxybut-1 -ene. The mixture is refluxed for 10 h, then treated with 100 ml methanol/water (1 1), and extracted with chloroform. The organic phase is separated, dried with anhydrous magnesium sulfate, filtered, and the filtrate evaporated. The residue is chromatographed on silica gel with chloroform as the mobile phase. The product is recrystallized from chloroform/petroleum ether (30-60°) yield 80% m.p. 90-92°. 

A nuclear magnetic resonance study ( H, Te) of these reaction mixtures established that ketonyl tellurium trichlorides and diketonyl tellurium dichlorides are present. The easily crystallized and less soluble compounds were isolated. Contrary to Morgan s claim, ethyl methyl ketone did react to give bis[2-oxo-l-butyl] tellurium dichloride albeit in very low yield. Alkyl ethyl ketones and tellurium tetrachloride produced very low yields of bis[3-oxo-2-alkyl] tellurium dichlorides. Cyclooctanone and tellurium tetrachloride in refluxing carbon tetrachloride gave bis[2-oxocyclooctyl tellurium dichloride (m.p, 174°) in 40% yield . 

Einen analogen Anwendungsbereich haben Kalium-tributyl-(2)- und Kalium-triiso-propyloxy-hydrido-borat5 (s. Tab. 28, S. 334) sowie Bis-[3-methyl-butyl-(2)]-boran6 (s. Tab. 24, 27, 28, S. 329, 330, 334). Mit letzterem erhalt man z. B. aus 2-Oxo-l-phenyl-cy-clopentan 73% d.Th. 2-Hydroxy-1-phenyl-cyclopentan6. 

Chlor-l-athoxycarbonylamino- 675 1 -Chlor-1 -butyl- 586 4-Chlor-4-methyl-l -tert.-butyl- 511 1-Chlor-l-nitro- 575 1-Chlor-1 -nitroso- 472 l-Chlor-2-oxo-l-athoxycarbonyl- 674 1-Cyanamino-1,2-dimethyl-105 Cyan- 109, 587 1 -Deutero-l-methyl-... 

Pent-2-en-4-olide, 3-iso-propyl Lf 0.008 Pent-2-en-4-olide, 4-methyl-3-(3-oxo-l-butyl) Lf 0.005NT549... 

To a mixture of 4.4 parts of 4-(2-oxo-l-benzimidazolinyl)-piperidine, 3.3 parts sodium carbonate, a few crystals of potassium iodide in 200 parts 4-methyl-2-pentanone are added portionwise 6.2 parts l-chloro-4,4-di-(4-fluorophenyl)-butane. After the addition is complete, the whole is stirred and refluxed for 65 hours. After cooling the reaction mixture, there are added 70 parts water. The organic layer is separated, dried over potassium carbonate, filtered and evaporated. The solid residue is triturated in diisopropyl-ether, filtered off again and recrystallized from a mixture of 120 parts acetone and 80 parts 4-methyl-2-pentanone, yielding the crude product. After recrystallization of this crop from 80 parts acetone, l-[4,4-di-(4fluorophenyl)-butyl]-4-(2-oxo-l-benzimidazolinyl)-piperidine is obtained, melting point 217°C to 219°C. 

Bromo-1,8-naphthyridin-4( l//)-one 7-Bromo-2-phenyl-1,8-naphthyridi n-4( 1H)-one Butyl 4-amino-l-ethyl-2-oxo-l,... 

Chloro-2-[4-[4-(2H-benzimidazo-2-oxo-l-yl)piperidin-l-yl]butyl]-2H-thieno[3,2-e]-l,2-thiazine 1,1-dioxide hydrochloride, (V), and related 5HT7 receptor agonists prepared by May (5) were effective in the treatment of circadian rhythm disorders. 

Dimethyl-5-ethoxycarbonyl-E16c, 122 (En-azid/Ringschl.) Pyrido[3,4-d pyridazin 1,4-Diethoxy-E9c, 68 (Cl - OR) Pyrido[2,3-d(pyrimidin 1 -Butyl-4-hydroxy-2-oxo-l,2-dihydro- E9c, 97 (2-NH R — 3-COOH—py + Urea)... 

Imidazolidin 3,4-Dimethy]-2-oxo-l-phenyl- E4, 376 (Umamidier.) lH-lndazol l-Butyl-3-hydroxy- E8b, 791 (Ar—NR —CO —Cl 4-NaN3)... 

Dithian 2-(2-Oxo-l, 1,3-trime-thyl-butyl)- E14a/3, 475 (1,3-Dithian-2-ylium +... 

Glycyl-L-leucine Glyoxal 1 -(1 -Carboxy-3 -methy 1-butyl)-2-oxo-l, 2-dihydro 380... 

In 23-dihydroxypyrazine and derivatives Honzl (853), from measurements of infrared spectra in chloroform and ultraviolet spectra in aqueous alcohol, has proposed that 5,6-dichloro-l-cyclohexyl-3-hydroxy-2-oxo-l, 2-dihydropyrazine (pA in water 4.66, 5.66) exists in the form (48). The p.m.r. spectra of some 5- and 6-methyl- and 5- and 6-phenyl-2,3-dihydroxypyrazines have been reported (483). In the 2,5-dihydroxypyrazine series, the infrared spectrum (Nujol) of 2-benzyl-3,6-dihydroxy-5-methylpyrazine has been interpreted as indicating that the major tautomeric form present in the solid state was the dihydroxy form (49), but the ultraviolet spectrum in ethanol was considered consistent with the coexistence of the dihydroxy (49) and oxo-hydroxy form, for example, (50), Although the structure (51) has been proposed for 3-butyl-2,5-dihydroxypyrazine (1092), the evidence in favor of this structure is inconclusive. 

Piperazin-2-one with benzyl chloride and sodium carbonate gave 4-benzyl-piperazin-2-one, which with acrylonitrile gave 4-benzyl-l-cyanoethylpiperazin-2-one or with butyl bromide and sodium in toluene formed 4-benzyl-1-butylpiperazin-2-one (1615) but (Z)-3-benzylidene-l-methylpiperazine-2,5-dione methylated with methyl iodide and silver carbonate produced (Z)-3-benzylidene-5-methoxy-1 -methyl-2-oxo-l,2,3,6-tetrahydropyrazine (88) and a small amount of (Z)-3-benzylidene-l,4-dimethylpiperazine-2,5-dione (89) (1616). 

Methyl-l-oxo- 2507 Cyclooctene 3-Methoxy- 2652 Cyclopropane 2-Acetyl-l-butyl- 2483... 

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