Dimethyl homophthalate condensed with isatin to give the unexpected five membered lactone 3 rather than the half ester 1 and the β-lactone 2. Treatment of compound 3 with excess hydrazine hydrate afforded phthalazino...Dimethyl homophthalate condensed with isatin to give the unexpected five membered lactone 3 rather than the half ester 1 and the β-lactone 2. Treatment of compound 3 with excess hydrazine hydrate afforded phthalazinone carbohydrazide 4 which represents a novel method for the synthesis of phthalazinone derivatives. The carhohy- drazide 4 upon treatment with carbon disulphide afforded 1,3,4-oxadiazole derivative 5, which reacted with ethyl- chloroacetate to give the S-alkylated product 6. The structure of compound 3 compared with 2 was discussed using hyperchem professional （7） AM1 calculations, X-ray single crystal structure and complete spectral data.展开更多
A facile synthesis of 2,2-disubstituted idanes was achieved by the reductive cyclization of 1-(o-bromomethylphenyl)-2,2-disubstituted-ethylenes(electron-withdrawing substituents) with an NAD(P)H model, 1-benzyl-1,4-di...A facile synthesis of 2,2-disubstituted idanes was achieved by the reductive cyclization of 1-(o-bromomethylphenyl)-2,2-disubstituted-ethylenes(electron-withdrawing substituents) with an NAD(P)H model, 1-benzyl-1,4-dihydronicotinamide, in yields from moderate to good. The study revealed that \{1-benzyl\}-1,4-dihydronicotinamide can be used in synthetic organic chemistry as an effective reductant.展开更多
2,6-Diisopropylnaphthalene （2,6-DIPN）, as the precursor of important monomer 2,6-naphthalene dicarboxylic acid, could be produced by the shape-selective isopropylation of naphthalene with propene resulting in an iso...2,6-Diisopropylnaphthalene （2,6-DIPN）, as the precursor of important monomer 2,6-naphthalene dicarboxylic acid, could be produced by the shape-selective isopropylation of naphthalene with propene resulting in an isomeric mixture having different alkylation levels. Since the boiling points of DIPNs were very close and the differences of melting points in-between isomers were quite distinctive, the static melt crystallization was applied to separate and purify 2,6-DIPN from its isomers. 2,6-DIPN with purity ≥99% was produced through a process of three stages： crystallization→sweating→melting. The phase diagram of 2,6-DIPN-2,7-DIPN binary system was plotted to opti- mize the temperature control of crystallization. By repeated crystallization of melts with different concentration levels, the yield of pure 2,6-DIPN could be enhanced to 87%. No solvent was necessary. Keywords 2,6-diisopropylnaphthalene, static melt crystallization, crystallization rate, sweating rate, eutectic temperature展开更多
文摘Dimethyl homophthalate condensed with isatin to give the unexpected five membered lactone 3 rather than the half ester 1 and the β-lactone 2. Treatment of compound 3 with excess hydrazine hydrate afforded phthalazinone carbohydrazide 4 which represents a novel method for the synthesis of phthalazinone derivatives. The carhohy- drazide 4 upon treatment with carbon disulphide afforded 1,3,4-oxadiazole derivative 5, which reacted with ethyl- chloroacetate to give the S-alkylated product 6. The structure of compound 3 compared with 2 was discussed using hyperchem professional （7） AM1 calculations, X-ray single crystal structure and complete spectral data.
文摘A facile synthesis of 2,2-disubstituted idanes was achieved by the reductive cyclization of 1-(o-bromomethylphenyl)-2,2-disubstituted-ethylenes(electron-withdrawing substituents) with an NAD(P)H model, 1-benzyl-1,4-dihydronicotinamide, in yields from moderate to good. The study revealed that \{1-benzyl\}-1,4-dihydronicotinamide can be used in synthetic organic chemistry as an effective reductant.
文摘2,6-Diisopropylnaphthalene （2,6-DIPN）, as the precursor of important monomer 2,6-naphthalene dicarboxylic acid, could be produced by the shape-selective isopropylation of naphthalene with propene resulting in an isomeric mixture having different alkylation levels. Since the boiling points of DIPNs were very close and the differences of melting points in-between isomers were quite distinctive, the static melt crystallization was applied to separate and purify 2,6-DIPN from its isomers. 2,6-DIPN with purity ≥99% was produced through a process of three stages： crystallization→sweating→melting. The phase diagram of 2,6-DIPN-2,7-DIPN binary system was plotted to opti- mize the temperature control of crystallization. By repeated crystallization of melts with different concentration levels, the yield of pure 2,6-DIPN could be enhanced to 87%. No solvent was necessary. Keywords 2,6-diisopropylnaphthalene, static melt crystallization, crystallization rate, sweating rate, eutectic temperature
