The first X-ray crystal structure determination of a thiosulphite 00'-diester is reported.THE branch-bonded sulphur species (1) were initially considered as structures for the disulphides (2) and trisulphides ( 3 ) 2 and have been suggested as reactive intermediates in S If RS-SR S II S

No abstract

No abstract

3) s, 8.15 (3) m, and 8.30 (3) m as the major peaks; ultraviolet spectrum: XXmax 279 µ (e 7000) and 522 µ (e 29) (the extinction coefficients are based on an estimated 60% conversion); infrared spectrum: 2035 cm-1 (C=N=N). Part of the reaction mixture was added to an ethereal solution of benzoic acid. Nitrogen was evolved and the solution decolorized. The mixture was washed with sodium bicarbonate and water. After evaporation of the solvent, the residue was distilled under vacuum (60°(0.5 mm)). The distillate gave infrared and nmr spectra identical with those obtained from a sample of 2-methyl-4-benzoyloxy-2-pentene.2-Methyl-4-benzoyloxy-2-pentene. 2-Methyl-2-penten-4-ol (12 g, 0.12 mole) was allowed to react with benzoyl chloride (16.8 g, 0.12 mole) in pyridine (100 ml) at 0°for 40 min. The reaction mixture was poured on ice, extracted with ether, and dried over sodium sulfate. Distillation yielded a fraction (13.35 g) boiling at 60-80°( 0.025 mm) consisting mainly of benzoate. Repeated distillation over a column gave a pure sample boiling at 62 °(0.05 mm).Anal. Caled for Ci3Hi602: C, 76.44; H, 7.84. Found: C, 76.26; H, 7.84. l-Phenyl-l-diazo-3-methyl-2-butene from 3,3-Dimethyl-5-phenyl-3/f-pyrazole. 3/7-Pyrazole IV (1.27 g, 7.4 mmoles) in methylene chloride (100 ml) was irradiated at -40°u sing apparatus B equipped with Corning filter 7-37. No nitrogen evolution was detected. After 80 min, the irradiation was discontinued, and a sample of the solution was analyzed by nmr: 2.7 (5) (m), 7.98 (3) m, and 8.22 (3) m. Based on an integration of the nmr peaks conversion to the diazo compound was 86%; ultraviolet spectrum: XXmax 292 µ (e 18,000) and 522 µ (c 56) (the extinction coefficients are based on the conversion as determined by nmr); infrared spectrum: 2035 cm-1 (C=N=N).

No abstract