secondary cells with lithium anodes and immobilized fused_salt

60.
identified (Reference 7) as the FEFO analogs with two and three methy’leneoxy chafns
in the molecule, respectively.
V VI
Compounds V and VI seem to arise whenever the condensation medium is contaminated with
water. If one is aware of this beforehand, the problem can be overcome by the use of
fuming sulfuric acid, as shown i n Table 2.
TABLE 2
,
EFFECT OF DILUTION WITH WATER ON FEFO SYNTHESIS
~o10-s Components
Case
No. Condi tions
with lower CC
retention time $ FEFO $ *ah-boilers $ Yield
-
5 Standard* 3.6 93.4 3-0 92.5
6 IO$ H20 added to PDNE 4.3 44.7 51.0 83.6
7 As in 93, with 20-29 2.9 93.4 3.7 77.7
fuming &SO4 in place of
conc. H SO
2 4
2.0 moles of FDNE (distilled) per mole of formaldehyde
Results similar to those of Case No. 6 are obtained whenever the FDNE-methylene chlorido
solutions are inadequately dried.
If the FEFO product is still too highly Contaminated with V and/or VI, purifica-
tion may be effected by low-temperature crystallization from methylene chloridchexane
in a tedious, somewhat wasteful procedure, or by agitation with concentrated sulfuric
acid. Result5 from the latter treatment are presented in Table 3. m
TABLE 3
PURIFICATION OF FEFO WITH SULFURIC ACID
,
Case
No.
8, crude
#ole-% Components
with lower CC
retention time $ FEFO
1.2 87.3
$ Eiph-Boilers
--
v VI $ Recovery
5.6 5.9 -
8, purified
9, crude
9, purified
1.7
0.7
1-4
96.6
95.6
98-6
0.1
3.7 -
1.6
-
82
- -
89 I1
Extremely interesting results were obtained in the course of preparing FEFO from
an FDNE-methylene chloride solution after attempted purification. This FDNE was prepared
fro= f luorotrinitromethans in aethanolic solution. and the FDmmethylene
chloride solution was later found to be highly contaminated with methanol and water.
The crude FEFSmethylene chloride solution, following separation from the sulfuric
acid layer, was divided into two equal portions. One portion was worked up in tho
usual manner, and the other waa treated with two portions of concentrated sulfuric
1
4
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i
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