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Inorganic microsynthesis
130
ABSTRACTS
Isotope dilution method for assay of inayylutinable erythrocytes, K. C. Atwood and S. L. Scheinberg, Science, 129,963-64 (1959). The true inagglutinable proportion of cells can be found by successive agglutinat,ions of a labeled population in the presence of unlabeled carrier cells. Free p-hydroxy-r-aminobutyric acid in brain, K. Ohara, Science, 129, 1225-26 (1959). @Hydroxy-r-aminobutyric acid was shown to exist in the brain of mice, rabbits, cattle, and humans by comparing the patterns obtained in paper chromatography and high-potential paper electrophoreeis of prepared extracts with those obtained with synthetic acid. Use of phosphorus-32 in microassay for nucleic acid synthesis in Escherichia coli, P. Hanawalt, Science, 130, 386-U (1959). A rapid means of determining less than 1 pg. ribonucleic acid and deoxyribonucleic acid in bacterial cultures is described. A modified Schmidt-Thannhauser procedure is applied to microquantities of Pa2 labeled cells collected on a membrane. Identi$cation Hendershott flavanone is point, paper
of a growth inhibitor from extracts of dornkant peach$ower buds, C. H. and D. R. Walker, Science, 130,798-99 (1959). 5,7,4’-Trihydroxyisolated and identified by infrared and ultraviolet spectra, melting chromatography, and activity in the bioassay test.
A nkicrowlorimetric method for the determination of antimony in biological material, C.-K. Ho, C.-C. Kung, S.-y. Wang, and L. Li, Sheng Li Hsueh Pao, 21, 167-73 (1957). The sample is digested, later extracted and red color formed with Rhodamine B is measured spectrophotometrically.
Inorganic Microsynthesis Diphenylacetylene derivatives of iron carbonyl, G. N. Schrauzer, J. Am. Chem. Sot., 81, 5307-10 (1959). The conversion of 72-100 mg. iron carbonyl complexes by thermal decomposition and by base is described. Substituted carbonyl compounds of chromium, molybdenum, tungsten, and mangarzese, E. W. Abel, M. A. Bennett, and G. Wilkinson, J. Chem. Sot., 1959, 232327. Complexes of the type L,M(CO)I, where M is (Cr, MO, W), and L represents various N, P, As, and Sb donor compounds have been synthesized in decigram quantities. Phosphine complexes of di- and trivalent chromium, K. Isslieb and H. 0. FrShlich, 2. anorg. u. allgem. Chem., 298, 84-99 (1959). Preparation of CrC& [P(C&H&]2 from 300 mg. CrCl* and 300 mg. P(C2H& in anhydrous benzene is described. (See specifically p. 98). On the action of halogenates on vanadium(IZZ) oxide in aqueous solution, T. Kuusinen, 2. anorg. u. &gem. Chem., 298,194-201(1959). Investigation of theprodMlCROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1
131
ABSTRACTS ucts obtained by the action of alkali metal chlorate, bromate, perchlorate on 200-mg. quantities of V203 is reported.
iodate, periodate,
or
Preparation of chromium(~ll)-tris(8-amino-ethylate), A. Kiintael and H. Trabitzsch; Z. unurg. u. allgem. Chem., 299, 188-196 (1959). Preparation and purification of red crystalline Cr(OCH&H,NH& for microscopic investigation is described. On the reaction IlNb + Z&O2 + 6NbO + NbsSi3, H. Schafer and K. D. Dohmann, Z. anorg. u. allgem. Chem., 299, 197-202 (1959). The preparation of Nb&& by heating 400 mg. Nb powder and SiO, in a sealed evacuated quartz tube at 8001000” for several days is described. Preparative studies with lower niobium chlorides, H. Schafer and K. D. Dohmann, Z. arwrg. u. allgem. Chem., 300, l-32 (1959). Preparations of decigram quantities of niobium chlorides in a sealed tube are described.
Organic Microsynthesis Synthesis of da-methyl-ALsteroids. The interrelationships of cholesterol, citrostdienol, and lophenol, Y. Mazur and F. Sondheimer, J. Am. Chem. Sot., 80,629699 (1958). Descriptions are given of the modification of the Wolff-Kishner reduction, oxidation, and ozonolysis procedures for use with 15-500 mg. of steroid. and structure of the Co, unsaturated fatty acids in menhaden body oil, W. Stoffel and E. H. Ahrens, Jr., J. Am. Chem. Sot., 80,6604-6608 (1958). Adaptations of oxidation and reductive ozonolysis procedures for 25-100 mg. fatty acid are des,cribed.
Isolation
The synthesis of d-(Ghydroxy-d-methoxy-S,(t-methylene dioxyphenyl)-benzojuran, a new compound from yeast, A. F. Wagner, A. N. Wilson, and K. Folkers, J. Am. Chem. Sot., 81, 5441-44 (1959). Fusion of 16 mg. of 2-(2methoxy-3,4-methylenedioxyphenyl)3-nitrofuran, 125 mg. of KOH, and 2 drops of water in a gold crucible at 230” yields 4.8 mg. product after purification. (See specifically p. 5444.)
Reaction of diazomethane with A%!?O-ketosteroids, H. L. Slates and N. L. Wendler, J. Am. Chem. Sot., 81, 5472-75 (1959). KMn04 and 050a oxidation, maleic anhydride addition, formylation, and isomerization of IO-100-mg. quantities of the ketosteroids are described. Thiohydantoins. Part IV, J. T. Edward and S. Nielsen, J. Chem. Sot., 1959,232731. Oxidation and acid and alkaline hydrolysis of decigram quantities of thiohydantoins are reported.
ABSTRACTS
Isotope dilution method for assay of inayylutinable erythrocytes, K. C. Atwood and S. L. Scheinberg, Science, 129,963-64 (1959). The true inagglutinable proportion of cells can be found by successive agglutinat,ions of a labeled population in the presence of unlabeled carrier cells. Free p-hydroxy-r-aminobutyric acid in brain, K. Ohara, Science, 129, 1225-26 (1959). @Hydroxy-r-aminobutyric acid was shown to exist in the brain of mice, rabbits, cattle, and humans by comparing the patterns obtained in paper chromatography and high-potential paper electrophoreeis of prepared extracts with those obtained with synthetic acid. Use of phosphorus-32 in microassay for nucleic acid synthesis in Escherichia coli, P. Hanawalt, Science, 130, 386-U (1959). A rapid means of determining less than 1 pg. ribonucleic acid and deoxyribonucleic acid in bacterial cultures is described. A modified Schmidt-Thannhauser procedure is applied to microquantities of Pa2 labeled cells collected on a membrane. Identi$cation Hendershott flavanone is point, paper
of a growth inhibitor from extracts of dornkant peach$ower buds, C. H. and D. R. Walker, Science, 130,798-99 (1959). 5,7,4’-Trihydroxyisolated and identified by infrared and ultraviolet spectra, melting chromatography, and activity in the bioassay test.
A nkicrowlorimetric method for the determination of antimony in biological material, C.-K. Ho, C.-C. Kung, S.-y. Wang, and L. Li, Sheng Li Hsueh Pao, 21, 167-73 (1957). The sample is digested, later extracted and red color formed with Rhodamine B is measured spectrophotometrically.
Inorganic Microsynthesis Diphenylacetylene derivatives of iron carbonyl, G. N. Schrauzer, J. Am. Chem. Sot., 81, 5307-10 (1959). The conversion of 72-100 mg. iron carbonyl complexes by thermal decomposition and by base is described. Substituted carbonyl compounds of chromium, molybdenum, tungsten, and mangarzese, E. W. Abel, M. A. Bennett, and G. Wilkinson, J. Chem. Sot., 1959, 232327. Complexes of the type L,M(CO)I, where M is (Cr, MO, W), and L represents various N, P, As, and Sb donor compounds have been synthesized in decigram quantities. Phosphine complexes of di- and trivalent chromium, K. Isslieb and H. 0. FrShlich, 2. anorg. u. allgem. Chem., 298, 84-99 (1959). Preparation of CrC& [P(C&H&]2 from 300 mg. CrCl* and 300 mg. P(C2H& in anhydrous benzene is described. (See specifically p. 98). On the action of halogenates on vanadium(IZZ) oxide in aqueous solution, T. Kuusinen, 2. anorg. u. &gem. Chem., 298,194-201(1959). Investigation of theprodMlCROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
1
131
ABSTRACTS ucts obtained by the action of alkali metal chlorate, bromate, perchlorate on 200-mg. quantities of V203 is reported.
iodate, periodate,
or
Preparation of chromium(~ll)-tris(8-amino-ethylate), A. Kiintael and H. Trabitzsch; Z. unurg. u. allgem. Chem., 299, 188-196 (1959). Preparation and purification of red crystalline Cr(OCH&H,NH& for microscopic investigation is described. On the reaction IlNb + Z&O2 + 6NbO + NbsSi3, H. Schafer and K. D. Dohmann, Z. anorg. u. allgem. Chem., 299, 197-202 (1959). The preparation of Nb&& by heating 400 mg. Nb powder and SiO, in a sealed evacuated quartz tube at 8001000” for several days is described. Preparative studies with lower niobium chlorides, H. Schafer and K. D. Dohmann, Z. arwrg. u. allgem. Chem., 300, l-32 (1959). Preparations of decigram quantities of niobium chlorides in a sealed tube are described.
Organic Microsynthesis Synthesis of da-methyl-ALsteroids. The interrelationships of cholesterol, citrostdienol, and lophenol, Y. Mazur and F. Sondheimer, J. Am. Chem. Sot., 80,629699 (1958). Descriptions are given of the modification of the Wolff-Kishner reduction, oxidation, and ozonolysis procedures for use with 15-500 mg. of steroid. and structure of the Co, unsaturated fatty acids in menhaden body oil, W. Stoffel and E. H. Ahrens, Jr., J. Am. Chem. Sot., 80,6604-6608 (1958). Adaptations of oxidation and reductive ozonolysis procedures for 25-100 mg. fatty acid are des,cribed.
Isolation
The synthesis of d-(Ghydroxy-d-methoxy-S,(t-methylene dioxyphenyl)-benzojuran, a new compound from yeast, A. F. Wagner, A. N. Wilson, and K. Folkers, J. Am. Chem. Sot., 81, 5441-44 (1959). Fusion of 16 mg. of 2-(2methoxy-3,4-methylenedioxyphenyl)3-nitrofuran, 125 mg. of KOH, and 2 drops of water in a gold crucible at 230” yields 4.8 mg. product after purification. (See specifically p. 5444.)
Reaction of diazomethane with A%!?O-ketosteroids, H. L. Slates and N. L. Wendler, J. Am. Chem. Sot., 81, 5472-75 (1959). KMn04 and 050a oxidation, maleic anhydride addition, formylation, and isomerization of IO-100-mg. quantities of the ketosteroids are described. Thiohydantoins. Part IV, J. T. Edward and S. Nielsen, J. Chem. Sot., 1959,232731. Oxidation and acid and alkaline hydrolysis of decigram quantities of thiohydantoins are reported.