1968
DOI: 10.1002/ange.19680801514
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Phosphor(v)‐isocyanate

Abstract: Vor kurzem berichteten wir "1 uber eine einfache Methode zur Synthese von Phosphor-und Thiophosphorsaure-diesterisocyanaten (2) durch Einwirkung von Oxalsauredichlorid auf entsprechende Phosphorsaure-diester-amide (I). Die Reaktion fuhrt man in inerten Losungsrnitteln (2.B. CC14, Benzol) bei 0 "C durch.

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“…The 1-H cation 4d was also present (on average ca. 20%, its low-field signals being recorded first were weaker than the high-field signals): 1.57 (d, J = 7.0 Hz, 3 H, 1-Me), 2.69 (3 H, 3-Me), 2.96 (3 H, 6-Me), 4.05 (q, J = 7.0 Hz, 1 H, 1-methine), 7.57 (5 H, 2-Ph), 8.16 (d, J = 9.0 Hz, 1 , H-7), and 8.54 (d, J = 9.0 Hz, 1 H, H-8); pmr (CFg-COOD) 1.56 (3 H, 1-Me), 2.69 (3 H, 3-Me), 2.96 (3 H, 6-Me), 5.75 (5 H, 2-Ph), 8.16 (d, J = 9.0 Hz, 1 , H-7), and 8.54 (d, J = 9.0 Hz, 1 , H-8). This first recorded spectrum of the perchlorate of 2f, when retraced after a further 5 min, showed a marked increase in the concentration of the 1-H cation 4d (55%) and the emergence of the 3-H cation 3d (20%).…”
Section: Methodsmentioning
confidence: 95%
“…The 1-H cation 4d was also present (on average ca. 20%, its low-field signals being recorded first were weaker than the high-field signals): 1.57 (d, J = 7.0 Hz, 3 H, 1-Me), 2.69 (3 H, 3-Me), 2.96 (3 H, 6-Me), 4.05 (q, J = 7.0 Hz, 1 H, 1-methine), 7.57 (5 H, 2-Ph), 8.16 (d, J = 9.0 Hz, 1 , H-7), and 8.54 (d, J = 9.0 Hz, 1 H, H-8); pmr (CFg-COOD) 1.56 (3 H, 1-Me), 2.69 (3 H, 3-Me), 2.96 (3 H, 6-Me), 5.75 (5 H, 2-Ph), 8.16 (d, J = 9.0 Hz, 1 , H-7), and 8.54 (d, J = 9.0 Hz, 1 , H-8). This first recorded spectrum of the perchlorate of 2f, when retraced after a further 5 min, showed a marked increase in the concentration of the 1-H cation 4d (55%) and the emergence of the 3-H cation 3d (20%).…”
Section: Methodsmentioning
confidence: 95%
“…7 In distinction to the mass spectral behavior of pyridine,8 however, the completely phenylated derivatives of pyridine, pyrazine, and 1,2,4-triazine were found not to scramble appreciably before decomposition. 4 We therefore thought it of interest to examine the extent of scrambling before fragmentation for several fully phenylated five-membered heterocycles containing nitrogen. This report is concerned with the scrambling in various fragment ions…”
Section: Methodsmentioning
confidence: 99%