For distillation of solids

The apparatus for distillation of solids in vacuum described in Organic Syntheses is satisfactory, as is a combination of standard taper flasks, short column, and adaptors. 

The crude product is then transferred to an apparatus suitable for distillation of solids (Note 6), and this is joined to a high-vacuum system capable of a vacuum in the range of 10 2 5 mm. Distillation begins when the bath temperature reaches about 190° a boiling point of around 120° is usually observed. When the distillate first begins to appear brown rather than violet, the distillation is stopped immediately (Note 7). The crystalline distillate (ca. 70 g.) is dissolved in 20 ml. of hot ethanol, filtered while hot, and allowed to cool. The solid (about 60 g. of crystals, m.p. 74—76°) is recrystallized from 20 ml. of ethanol to yield 47-53 g. (43-49%) of 4,6,8-trimethylazulene as dark-violet plates, m.p. 80-81° (Note 8). 

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