Phosphorus colourless

TC. Colourless gas obtained from elements in presence of a catalyst (charcoal or Pt) or from Bra, red phosphorus, and H2O (HBr... 

Phosphine is a colourless gas at room temperature, boiling point 183K. with an unpleasant odour it is extremely poisonous. Like ammonia, phosphine has an essentially tetrahedral structure with one position occupied by a lone pair of electrons. Phosphorus, however, is a larger atom than nitrogen and the lone pair of electrons on the phosphorus are much less concentrated in space. Thus phosphine has a very much smaller dipole moment than ammonia. Hence phosphine is not associated (like ammonia) in the liquid state (see data in Table 9.2) and it is only sparingly soluble in water. 

Phosphorus trifluoride is a colourless gas the molecule has a shape similar to that of phosphine. Although it would not be expected to be an electron donor at all (since the electronegative... 

Arsenic forms only the pentafluoride AsFj, a colourless liquid, b.p. 326 K. This resembles phosphorus pentafluoride. 

Assemble in a fume-cupboard the apparatus shown in Fig. 67(A). Place 15 g. of 3,5-dinitrobenzoic acid and 17 g. of phosphorus pentachloride in the flask C, and heat the mixture in an oil-bath for hours. Then reverse the condenser as shown in Fig. 67(B), but replace the calcium chloride tube by a tube leading to a water-pump, the neck of the reaction-flask C being closed with a rubber stopper. Now distil off the phosphorus oxychloride under reduced pressure by heating the flask C in an oil-bath initially at 25-30, increasing this temperature ultimately to 110°. Then cool the flask, when the crude 3,5-dinitro-benzoyl chloride will solidify to a brown crystalline mass. Yield, 16 g., i.e,y almost theoretical. Recrystallise from caibon tetrachloride. The chloride is obtained as colourless crystals, m.p. 66-68°, Yield, 13 g Further recrystallisation of small quantities can be performed using petrol (b.p. 40-60°). The chloride is stable almost indefinitely if kept in a calcium chloride desiccator. 

Trimethylene Di-iodide. Use 76 g. of trimethylene glycol, 27 - 52 g. of pmified red phosphorus and 254 g. of iodine. Lag the arm C (Fig. Ill, 40, ) with asbestos cloth. Stop the heating immediately all the iodine has been transferred to the fiask. Add water to the reaction mixture, decolourise with a httle sodium bisulphite, filter, separate the crude iodide, wash it twice with water, dry with anhydrous potassium carbonate and distU under reduced pressure. B.p. 88-89°/6 mm. Yield 218 g. (a colourless liquid). 

Place 45 g. of benzamide (Section IV, 188) and 80 g. of phosphorus pentoxide in a 250 ml. Claisen flask (for exact experimeutal details on the handling and weighing out of phosphoric oxide, see under Acetamide, Section 111,111). Mix well. Arrange for distillation (Fig.//, 29, 1 or Fig. II, 20, 1) under reduced pressure use a water pump with an air leak in the system so that a pressure of about 100 mm. is attained. Heat the flask with a free flame until no more liquid distils the nitrile will pass over at 126-130°/100 mm. Wash the distillate with a little sodium carbonate solution, then with water, and dry over anhydrous calcium chloride or magnesium sulphate. Distil under normal pressure (Fig. II, 13, 2 or II, 13, 6) from a 50 ml. flask the benzonitrile passes over as a colourless liquid at 188-189° (compare Section IV,66). The yield is 28 g. 

Dinitrito - tetrammino - iridium Bromide, [Ir(NH3)4(N02)2] Br.H20, separates in long, colourless, flat prisms, and may be obtained anhydrous by reerystallisation from hydrobromic-acid solution. The hydrated salts lose water on heating but not over phosphorus pentoxide. 

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