3- Phenyl-2,4-pentanedione, from

Silver fluoborate, reaction with ethyl bromide in ether, 46, 114 Silver nitrate, complexing with phenyl-acetylene, 46, 40 Silver oxide, 46, 83 Silver thiocyanate, 45, 71 Sodium amide, in alkylation of ethyl phenylacetate w ith (2-bromo-ethyl)benzene, 47, 72 in condensation of 2,4-pentanedione and 1 bromobutane to give 2,4-nonanedione, 47, 92 Sodium 2 ammobenzenesulfinate, from reduction of 2 mtrobenzenesul-finic acid, 47, 5... 

Trimethyl phosphite (11.3 g, 0.091 mol) was added to a solution of 3-benzylidene-2,4-pentanedione (16.35 g, 0.091 mol) in dry methylene chloride. The solution was maintained under nitrogen for 24 h at 20°C and for an additional 5 h at 40°C. After this time, the solvent was evaporated, and the residue was dissolved in hexane. These actions were performed in the absence of moisture. The clear hexane solution was seeded with a crystal of the pure crystalline product (obtained by crystallization from hexane by standing for 2 weeks at 0°C), and after 8 h at 0°C the crystals precipitated yielding pure 2,2,2-tri-methoxy-3-phenyl-4-acetyl-5-methyl-A4-oxaphospholene (25.12 g, 88.4%) of mp 48-51°C. 

IODONIUM CHLORIDE 1-PHENYL-2, 4-PENTANEDIONE, 51, 128 4-Phenyl-l-carbethoxysemicar-bazide, from ethyl hydra-zinecarboxylate and phenyl isocyanate, 51, 122 with potassium hydroxide to give 4-phenylurazole, 51,... 

When a metal ion such as nickel (II) is absent, thiazoles and mercaptals are formed. Such reactions have been carried out in which the diketone was biacetyl, 2,3-pentanedione, 2,3-octanedione, l-phenyl-l,2-propane-dione, and 1,2-cyclohexanedione (51). In like manner, the tris complexes of W,W -dimethyl-2,3-butane diimine with iron(II), cobalt(II), and nickel(II) may be prepared from methylamine and biacetyl when the appropriate metal ion (27j 28j 41) is present. Replacing methylamine with hydroxylamine causes the formation of a-dioximes (13). 

Oxazolino-a-pyrone (487) was obtained in five steps starting from 3-benzo-yloxy-2,4-pentanedione (486). Catalytic hydrogenation of487 afforded two products with the same threo stereochemistry 3-benzamido-S-caprolactone (488) and an analogous compound (489) having the phenyl ring peihydrogenated. With... 

The 7-benzyl derivative of XII-53 (W-55) prepared from the sodium salt of 5-phenyl-l, 3-pentanedione, potassium amide, and methyl benzoate, was not isolated but was converted to S-benzyl-6-phenyl4-pyridone with ammonia in ethanol. " ... 

PBD-Modified LiNbOs Precursor. Non-modified LiNbOs (STD-LiNbOs) precursor solutions are prepared from LiOEt and Nb(OEt)s in ethanol (Hirano, 2002). The structure of the precursor was confirmed to consist of a complex alkoxide Li[Nb(OEt)6], which was reported by Eichorst et al. (1990) in detail (Eichorst et al., 1990). On the other hand, three types of/6-diketone compounds are selected based upon the number of benzene rings (phenyl groups) in its stmcture. In this case, the coordination of l-phenyl-1,3-butanedione (PBD) to the LiNbOs precursor is confirmed by UV spectra. The similar coordination is also realized in 2,4-pentanedione (PD)- and 1,3-diphenyl-1,3-propanedione (DPPD)-modified LiNbOs precursors, which was confirmed by UV-spectra. The proposed structures of these d-diketone modified LiNbOs precursors are shown in Figure 17-1. 

Europium acetate monohydrate (99.9 %), samarium acetate tetrahydrate (99.9 %), acetone-i 6 (D, 99.9 %) and CDCI3 (D, 99.8 %) were purchased from Wako Pure Chemical Industries Ltd. l,l,l,5,5,5-hexafluoro-2,4-pentanedione, 4,5-bis(diphenyl-pho-sphino)-9,9-dimethylxanthene, 4,5-bis(di-ferf-butylphosphino)-9,9-dimethylx-anthene and bis[(2-diphenylphosphino)phenyl]ether were obtained from Tokyo Kasei... 

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