Professional Documents
Culture Documents
(01. 260-551)
2
This invention relates to the preparation of ,
thioformamide by the reaction of formamide with
phosphorus pentasul?de in accordance with the
following equation:
and the product can be obtained in good yields 40 will result and the tendency for the product to
and purity. Other objects of the invention will
be contaminated with formamide will be in
be apparent from the following description.
creased. Larger amounts of the pentasul?de than
The above objects are accomplished in accord
those mentioned can be used but no particular
ance with the invention by reacting phosphorus
advantages result from such practice.
pentasul?de with formamide dissolved in tetra 45
When the reaction is carried out in the absence
hydrofuran. Formamide is soluble in tetrahydro
of a solvent for either reactant, the reaction is
furan in all proportions so that by the presence
frequently di?icult to start, but once started, it
of the latter in the reaction medium the form
usually proceeds too rapidly with formation of
amide will always be present in solution. This
is of considerable advantage when compared with 50 large amounts of by-products and with poor con
version to thioformamide. The use of tetrahy
the prior use of diethyl ether as reaction medium,
drofuran as a solvent for formamide in the reac
since formamide is practically insoluble in diethyl
tion mixture results in the reaction proceeding
ether and, therefore, the presence of the latter
smoothly and at a controllable rate with mark
does not facilitate the reaction between form
amide and phosphorus pentasul?de. The S0111 55 edly reduced amountof by-products and corre
2,682,558
3
spondinely increased conversion to thioform
amide. Ordinarily at least one part of tetra
hydrofuran will be employed for each part by
weight of formamide being reacted. Lesser
amounts of the solvent can be used but with
only minor advantages resulting. Amounts rang
ing from 1~20 parts by weight of the solvent
per part of formamide generally will be used.
Larger amounts of the solvent can be employed
Example 5
examples:
'
Example 1..
without puri?cation.
2,682,558
5
I claim:
amide employed.
Number
2,265,212
Name
Date
OTHER REFERENCES
Willstatter et al., Ber. deut. Chem, vol. 42
(1909), pp. 1911, 1912 and. 1920.