Organometallic Isocyanates and Isocyanurates of Groups IV and V¹

Abstract

Isocyanates 693 tion of di-( 1,1-dimethylbutyl) oxalate was dissolved in 2.5 ml. of ethyl acetate and placed in a 50-ml. erlenmeyer flask with 0.05 g. of hydrogenation catalyst (10% Pd on charcoal). The flask was attached to a low pressure hydrogenation apparatus and the mixture was stirred magnetically overnight at room temperature under 1 atm. of hydrogen pressure. After filtering, the solution was submitted to gas chromatographic analysis. In addition to the solvent peak only one more peak was obtained which had identical retention time with that of authentic 2-methylpentane.Gas chromatographic analyses were obtained from a Perkin-Elmer Model 154, an F and M Model 500, and a Beckman GC-2. All n.m.r. spectra were taken on an Varían A-60 n.m.r. spectrometer.Acknowledgment.-One of us, J. M. Corbett, thanks the Dow Chemical Company, Midland, Michigan, for a leave of absence and generous support during the summer of 1962.

Kinetics of bromination of benzene and methylbenzenes in acetic and trifluoroacetic acids

“…Chem., 8, 359 (1964). Received July 5,1967 The reaction of isocyanic acid with trifluoroacetic anhydride (eq 1) has been found to be a useful method for the preparation of trifluoroacetyl isocyanate and 2,2,2,2,,2',2,-hexafluorodiacetamide (perfluorodiacetamide). The relative yields of trifluoroacetyl iso-_.CF3C0NC0 + other products (CF3C0)20 + HNCO -<^( !)…”

Reaction of isocyanic acid with trifluoroacetic anhydride. Preparation of trifluoroacetyl isocyanate and 2,2,2,2',2',2'-hexafluorodiacetamide

“…Chem., 8, 359 (1964). Received July 5,1967 The reaction of isocyanic acid with trifluoroacetic anhydride (eq 1) has been found to be a useful method for the preparation of trifluoroacetyl isocyanate and 2,2,2,2,,2',2,-hexafluorodiacetamide (perfluorodiacetamide). The relative yields of trifluoroacetyl iso-_.CF3C0NC0 + other products…”

Synthesis and structure of μ-oxobis[(isocyanato)triphenylantimony] (1,4)-dioxane solvate

“…Reactions of organoantimony(V) compounds with urea have been described only in [1,2]. Thus, melting (130-140°C) tri-n-butyl-or triisobutylantimony dihydroxide or oxide with urea in a vacuum resulted in trialkylantimony diisocyanates [1].…”

“…Thus, melting (130-140°C) tri-n-butyl-or triisobutylantimony dihydroxide or oxide with urea in a vacuum resulted in trialkylantimony diisocyanates [1]. We have studied the interaction of tetraphenylantimony chloride and bromide with urea in the melt at 180°C.…”