Characteristic NMR Data

Tris(trimethylsilyl)phosphine is a colorless compound with a melting point near room temperature. Characteristic NMR data for a DME solution are 5,ih) 0.30 Jp = 4.4 cps 5,3ip,-251. In reactions with alcohols and water bis(trimethylsilyl) and (trimethylsilyl)phosphine can be synthesized acetyl chloride in a molar ratio of 1 3 gives triacetylphosphine. For the important reaction with 2,2-dimethylpropionyl chloride see Section 49. 

Lithium bis(trimethyIsiIyI)phosphide-bis(tetrahydrofuran) is a colorless crystalline compound that has been used by several research groups for introducing the bis(trimethylsiIyl)phosphinyl group. Characteristic NMR data of the THF solution are 0.53, = 4.0cps — 298. 

Summary The synthesis and characteristic NMR data of l,3-dineopentyl-pyrido[ft]-l,3,2 L -diazasilole are discussed. 

Some characteristic NMR data of 3 a-c are compiled in Table 1. Attempts to reduce these compounds to stable silylenes have met with limited success. So far, only the 1,3-dineopentyl-pyrido[6]-l,3,2X -diazasilole 4 has been obtained by stirring the 2,3-disubstituted pyridine derivative 3a with potassium for 2d at room temperature and could be isolated by sublimation at 115°C/10 mbar. The yield was low. 

IR data prove the expected cis arrangement of P and Si enforced by the chelating ligand for the complexes 2, while complexes 1 show the typical pattern of octahedral mono-phosphine complexes. Some characteristic NMR data are summarized in Table 1... 

In this section several characteristic NMR-data of 2-oxa-6-aza-adamantanes [X(2) = O, Y(6) = NR] diall be discussed standing as typical examples for the rather large number of 4,8-disubstituted 2,6-dihetero-adamantanes known so far. 

Tris(trimethylsilyl)phosphine is a colorless compound with a melting point near room temperature. Characteristic NMR data for a DME solution are 0.30 Jp (3ip)-251. In reactions with alcohols and water... 

Dimethyl-1 -(trimethylsiloxy)propylidene] (trimethylsilyl)phosphine is a yellow viscous liquid. Characteristic NMR data for a solution in benzene are (H3O3C Jp = 1.5 (HaOjSi-O 5, ,0.27 (HaQjSi-P... 

Table 1. Characteristic NMR data [ppm, Hz] for the X -phosphaalkyne Th MesSON-CsP and its derivatives.

Tetrasulfonated chiraphos is a white solid containing some residual sodium sulfate and should be stored under argon. It can be used directly as obtained as a ligand in homogeneous catalysis. The compound is soluble only in water. The characteristic NMR data are P NMR (D2O) d ppm — 9.6 NMR (D2O-f H2O2) phosphine oxide S ppm 14.5... 

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