Purification recrystallization

If the crude product melts lower, it contains too much tribromoaniline to permit satisfactory purification. Recrystallization effects no separation repeated fractional steam distillation is very slowly effective. 

Note 7). When the reaction has subsided, the oil bath is lowered and the condenser is removed. The flask is fitted for simple distillation, and ethyl bromide is distilled from the reaction mixture over a period of 3-4 hr by continued heating at 115°C (oil bath). The resulting light yellow oil is cooled to room temperature, whereupon it solidifies (Note 8). The crude product is collected by suction filtration and washed with three 100-nL portions of cold petroleum ether (bp 60-68°C) to give 50.1-56.3 g (80-90%) of diethyl phthalimidomethylphosphonate as white crystals, mp 60-63°C, which are used in the next step without further purification. Recrystallization of this material from diethyl ether/petroleum ether (bp 60-68°C) affords pure 3, mp 65-67°C (lit.,3 67 C) (Note 9). 

The product is of satisfactory purity for use in the 4,6,8-tri-methylazulene preparation without further purification. Recrystallization of a small sample of the 2,4,6-trimethylpyrylium perchlorate from a seven-fold amount of hot water, containing a few drops of perchloric acid and some carbon black, gives colorless crystals, m.p. 245-247° dec. However, the recrystallization of larger amounts in this way presents some hazard and is not recommended. Concentration of filtrates should be avoided (see Note 4). 

Purification recrystallization from ethyl acetate-hexane. Handling, Storage, and Precautions hygroscopic crystals. Use in a fume hood. 

Preparative Methods the phosphoramidite ligand can be prepared by the nucleophilic substitution of phosphory 1 chloride (formed from the reaction of PCI3 and (S)-2,2 -binaphthol in presence of triethylamine) with (R,R)-bis(l-phenylethyl)amine. Purification recrystallization from diethyl ether/dichloro-methane. 

Purification recrystallization from hexane, ethanol, or methanol/water. 

Method of purification Recrystallization from mixture of benzene and ligroin. 

Derivation Interaction of ammonium hydroxide and hydrofluoric acid with subsequent crystallization. Method of purification Recrystallization. 

What is the most likely outcome when a solution containing different molecular solutes is allowed to evaporate to dryness Unless a chemical reaction driven by the formation of covalent bonds takes place between the solutes, one would normally expect the appearance of separate molecular solids. This is a demonstration of the innate structural selfishness of molecules [60], and it is utilized every time recrystallization is employed as a method of purification. Recrystallizations are per-... 

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