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Volume 30, Issue 6
Displaying 1-12 of 12 articles from this issue
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Nobuo NAKABAYASHI1972 Volume 30 Issue 6 Pages 500-513
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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Recent Progress of Pigment Technology and Chemistry of PhthalocyaninesYoshié BANSHO1972 Volume 30 Issue 6 Pages 514-524
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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Susumu IWABUCHI, Kuniharu KOJIMA1972 Volume 30 Issue 6 Pages 525-538
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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Studies on the Reactions of Amines with Sulfur Trioxide IFujio KANETANI, Hachiro YAMAGUCHI1972 Volume 30 Issue 6 Pages 539-544
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
JOURNAL FREE ACCESSFor the purpose of determining the composition of the products in the reactions of lower aliphatic amines with sulfur trioxide, an analytical method was developed which was based on a combination of anion-exchange chromatographic separation and complexometric titration of components.
A reaction mixture obtained in the reaction of methylamine with sulfur trioxide was dissolved in water and diluted to 250 ml. An aliquot of this solution was applied upon an Amberlite CG-400 (Cl-form) column. Then, 0.15 M NaCl was passed through the column at a flow rate of 1.0 ml per min. N, N '-Dimethylsulfamide was first eluted, followed by N-methylsulfamate. Sulfate was then eluted with 0.5 M NaCl, and finally N-methylimidodisulfate with 1 M NaCl.
Each fraction was treated with 1 N HCl and 6 M NaNO2 solution. The sulfate ion formed was then precipitated in the usual manner by adding 0.01 M BaCl2, and after pH adjustment, the excess of barium ion was back-titrated in the presence of Zn-EDTA with 0.01M EDTA by use of Eriochrome Black T as an indicator.
This method proved to be simple, accurate and widely applicable.
Paper and thin-layer chromatography were also described.View full abstractDownload PDF (940K) -
Tatsuaki NAKAHARA, Hiromu YAMASHITA, Setsuji KOSA, Katsuta NAKAGAWA, M ...1972 Volume 30 Issue 6 Pages 545-548
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
JOURNAL FREE ACCESSIt is known that monosulfonation of 1-naphthol affords 1-naphthol-4-sulfonic acid along with 1-naphthol-2-sulfonic acid, but this reaction has not been applied to industrial preparations yet.
1-Naphthol was dissolved in an inert solvent such as ο-nitrotoluene, and less than 2 equivalents of sulfuric acid was added. The mixture was stirred for ca. 3 hours, and then poured into water.
The solvent was separated and KCl was added to the aqueous solution. The precipitated potassium 1-naphthol-2-sulfonate was filtered. Addition of NaCl to the filtrate yielded sodium 1-naphthol-4-sulfonate. The yield of potassium 1-naphthol-2-sulfonate and sodium 1-naphthol-4-sulfonate was 85-90%.
When the reaction was performed at higher temperatures in the range of-570°C, the yield of the 2-sulfonate decreased and that of the 4-sulfonate increased. Each crude product was purified by the salting-out method (more than 90% recovery and less than 0.5% contamination of the isomer).View full abstractDownload PDF (622K) -
Seisaku INADA, Akio SIBAZAKI, Yasu FURUKAWA, Mitsuo OKAZAKI1972 Volume 30 Issue 6 Pages 549-558
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
JOURNAL FREE ACCESS5, 9-Dimethyl-5, 6-dihydro- (or-5, 6, 8, 9-tetrahydro-) 4H-benzofuro- [5, 6, 7-de] isoquinoline-4, 6-dione (5a, 8a) were synthesized by the Claisen rearrangement of 4-allyloxynaphthal-N-methylimide. Similarly, 8-phenyl derivatives of (5a) and (8a), (5b, 8b) were obtained from 4-cinnamyloxynaphthal-N-methylimide. In addition to (8b), in the latter case, 5-methyl-8-phenyl-5, 6-dihydro-4 H, 10 H- [1] benzopyrano [6, 7, 8-de] isoquinoline-4, 6-dione (9) was formed as a by-product.
Furthermore, several 3-substituted-4-methoxynaphthal-N-methylimides [e. g. propenyl (11a), α-phenylpropenyl (11b), carboxy (12), methoxycarbonyl (13), carbamoyl (14) and benzoyl (16)] were derived from the 3-allyl- (10a) or 3-α-phenylallyl-4-methoxy derivative (10b). The fluorescence spectra of these compounds were determined and the relationship between their structures and spectra was discussed.
The results are as follows. 1) The annellated dihydrofuran ring (5a), (5b) causes a shift (30 mμ) to longer wavelength at the fluorescence maximum and a slight increase in the fluorescence intensity, compared with 4-methoxynaphthal-N-methylimide as the standard sample. 2) On the other hand, the annellated furan ring (8a) results in only 10mμ shift and its intensity falls to 1/10 of that of the standard sample. 3) Fluorescence intensities of (8b), (9), (11b) and (16) are too weak to be measured under the conditions probably due to the non-planarity between their phenyl group and the naphthalene nucleus.View full abstractDownload PDF (1915K) -
Kenji NEGORO, Kenichi SAIDA, Takashi SHIGEMI1972 Volume 30 Issue 6 Pages 559-562
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
JOURNAL FREE ACCESSSodium N-α-naphthylmethyl-sulfanilate (sample number, 1) and N, N-α, α-dinaphthylmethylsulfanilate (2) were obtained by reaction of α-chloromethylnaphthalene with sodium sulfanilate.
Their surface-active properties, surface tension, viscosity, electrolytic conductivity, solubilization, emulsification and wetting were examined.
Both samples exhibited considerable surface activities in surface tension, solubilization of Orange OT and emulsification of liquid paraffin in aqueous solution.
The curves of electrolytic conductivity as a function of concentration of samples, suggested the micelle formation for (2), but not for (1).View full abstractDownload PDF (575K) -
Yoshio ORITO, Osamu SABI1972 Volume 30 Issue 6 Pages 563-565
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
JOURNAL FREE ACCESSThe relation between the preparation conditions of supported ruthenium catalyst and the hydrogenation activity for benzene and acetone was investigated. The supports used were SiO2, Al2O3, and C. The hydrogenation was performed at 20°C (or 40°C) under the pressure of 4030kg/cm2. The catalysts were prepared by impregnating the supports with an agueous ruthenium chloride. The Ru-SiO2 and Ru-Al2O3 thus prepared are very preferable for the hydrogenation of benzene, but their activities for the acetone hydrogenation are low. In case of the acetone hydrogenation Ru-C is appropriate and a highly active catalyst is obtained by reducing it with hydrogen at 400500°C before hydrogenation.View full abstractDownload PDF (383K) -
Masayoshi OKANO, Takaaki ARATANI1972 Volume 30 Issue 6 Pages 566-570
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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[in Japanese]1972 Volume 30 Issue 6 Pages 574
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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[in Japanese], [in Japanese], [in Japanese]1972 Volume 30 Issue 6 Pages 574a-576
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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[in Japanese], [in Japanese]1972 Volume 30 Issue 6 Pages 576
Published: June 01, 1972
Released on J-STAGE: November 13, 2009
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