e 6G2 ) 



y^-iiitrofliioride is unaffGctcd lliercbv. Tliis did not seem to be quite 

 the case, so a small coiTectioii has to be applied: 



(/. 2.95 grams of pure i>N0o.C,;.H4.Fl were treated at 0° with iive times 

 the weight of faming nitric acid of 1.52 sp. gr. The compound rapidly dis- 

 solved without elevation of temperature. After one hour the liquid was 

 poured into ice water and the fluorine derivative was instantly precipitated 

 in a solid condition. When the liquid had become clear it was carefully 

 filtered and the mass was repeatedly triturated in ice water until the 

 acid reaction had completely disappeared. It was then treated with 9.65 cc. 

 of )/ Vo:; Na OCHs for 5 mmutes at lb''. The liquid was then titrated 



back with 4,77 cc. of n acid. This gives -^^ - 4.77 = 0.23 cc. of n alkali 



consumed, corresponding with 0.428 gram of dinitro compouud, or 1.4 "/o. 



b. 1.732 grams of the para compound were treated in the same manner. 

 But after the acid had been removed by washing, the residue was melted 

 to a clear liquid by applying a gentle heat. It w^as then cooled in ice water 

 and again triturated and washed in ice water until the last traces of acid 

 had disappeared: it was then treated as in a. 10.48 cc. of «,1.93 NaOCHs 

 were used and the liquid was titrated back with 5.3 cc. x acid; 0.1 cc. of 

 n alkali had therefore been absorbed corresponding v^'ith 0.186 gram of 

 dinitro compound or 1.0° 'q. The mean of the two determinations is there- 

 fore 1.2%. 



Beiiiji' in possession of these data, 1 ha\e now subjected the nitra- 

 tion product of l)enzene thioride to the same test. Dr. Beekman had 

 previously found that the nitration at with a mixture of 25 cc. 

 of nitric acid of 1.48 sp.p,T., 5 cc. acid of 1.51 sp. gr. and 10 grams 

 of benzene tluoride yields a compound consisting solely of mononitro 

 compound (to judge from its percentage of nitrogen; found 1;).95 

 calculated 9.93). I, therefore, nitrated in the same manner and puritied 

 the product, which in ice water is senii--solid, by first wasliing it 

 in ice water, being careful not to lose any oily globules, and thoi 

 with water at 20'', which caused the whole mass to melt to a homo- 

 genous liquid. After all acid reaction had disappeared the bulk of 

 the water was i-emoved by means of a separatory funnel, the clear 

 l)ale yellow oil was b-eed b-oni a few (b-ops of adhering water by 

 means of a strip of tilterpaper and the]i finally heated in a testtube 

 at 90° — 100' until it no longer became hazy on cooling. We may 

 assume that all the moisture has then been removed, likewise small 

 <(uaiitities of any niicliangcMlhenzeue fiuoride. The product so obtained 

 solidified after inoculation at 1<S^.7 ; a second preparation at 18'. (5. 



It docs m)t coutaiu Ueuzcue dinitrotluoride : 



1.4115 grams were treated for 5 minutes with 9.45 cc. of w Vi-gs «odium 

 meLhoxide. The liquid was titrated back with 4.9 cc. « acid, or 9.46 « 1.9s acid. 



