THE ESSENTIAL OIL, OF DORYPHORA SASSAFRAS. 275 



Determination of Camphor. — The portion boiling at 200 

 - 219° O. at 762 mm. was placed in a freezing mixture, and 

 the separated camphor pumped off, drained on a porous 

 plate, and purified by sublimation and recrystallisation from 

 alcohol. Over 40 grams of solid camphor were obtained 

 in this way. As thus separated, the purified material 

 possessed the following characters, viz: — 



Boiling point, 760° mm. 207° C. 



Melting point 176° C. 



2*2318 grams in 10 ccs. absolute alcohol gave [a] D 20° + 42° 



Oxime, melting point. 118-119° O. 



Determination of Safrol. — The remaining fractions dis- 

 tilling between 104 — 120° C. at 10 mm. were placed in a 

 bath of solid carbon dioxide, and the frozen mass trans- 

 ferred to a buchner filter funnel surrounded with a mixture 

 of ice and salt. On continued repetition of this process 

 about 250 ccs. of purified safrol were thus obtained. It 

 was washed with 3 % sodium hydroxide solution to remove 

 phenols, and again frozen, and subjected to distillation at 

 10 mm. On examination it gave the following character- 

 istics, viz: — 



Melting point +11° C. 



Boiling point 109-110° at 10 mm. 



Specific gravity at 15° O. 1*103 



Optical rotation +0*30° (due to slight impurity) 



Refractive index 20° O. 1*5375 



Its identity was confirmed by the preparation of the 

 following derivatives, piperonylic acid and heliotropine, viz: 



(1) 10 grams were shaken with 22 grams powdered 

 potassium permanganate and 3 grams potassium hydroxide, 

 700 ccs. water and 700 grams ice. On completion of the 

 reaction, removal of manganese sludge, and concentration 

 of the liquor, crystals of piperonylic acid were obtained in 

 excellent yield, on acidification with dilute sulphuric acid. 

 On recrystallisation from alcohol they melted at 228° O. 



