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Purification of Laboratory Chemicals, 8th Edition by W.L.F. Armarego

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In the second preparation tris[2-(methylamino)-ethyl]amine (1.67g, 11.4mmol), see [65604-89-9]) in CH2Cl2 (20ml) is added with stirring to a mixture of ClP(NMe2)2 (1.76g, 11.4mmol, TOXIC) and Et3N (1.5g, 15mmol) in CH2Cl2 (30ml) during 5 minutes, then the mixture is stirred at ~ 25° for 1 hour, the volatiles are evaporated off in vacuo to give the hydrochloride quantitatively. It can be recrystallised from hexane/CHCl3 (82% yield) in colourless crystals. When the hydrochloride salt is treated with AgBF4 in CH2Cl2 the HBF4 salt is obtained quantitatively. The salts are very difficult to deprotonate (see preceding entry). The X-ray crystal structure shows a short intra-annular bond between the apical N atom and the P atom with a robust P—H bond, ...

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