反応 #710515

ord-cc9e064660aa45cfb9a5b39058d818b9

反応方程式

CCNCC
diethylamine
CCC[NH+](CCC)CCC
tripropylammonium
CCN(CC)C(=S)S
diethyl dithiocarbamate
S=C=S
carbon disulfide
CCCN(CCC)CCC
tripropylamine
CCC[NH+](CCC)CCC.CCN(CC)C(=S)[S-]
final product
CCC[NH+](CCC)CCC.CCN(CC)C(=S)[S-]
Tripropylammonium N,N-Diethyl Dithiocarbamate

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is maintained at a temperature below 30° C
  2. 2
    その他to remove the excess amine
  3. 3
    その他for the removal of low volatiles

実験手順

Preparation of tripropylammonium salt of diethyl dithiocarbamate is as follows: 76 grams (1 mole) carbon disulfide and 143 grams (1 mole) tripropylamine are mixed at 10° C. under nitrogen. 80.5 grams (1.1 mole) diethylamine is added slowly and drop wise to the mixture and the mixture is maintained at a temperature below 30° C. Then the mixture is heated to 50° C. for 1 hour. The solution is then stripped out under vacuum to remove the excess amine and for the removal of low volatiles to obtain final product. The acid number (normally below 30) is measured to check the acidity. The product purity (ranging between 85-95%) is measured by LC-MS and NMR.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09302272B2uspto-grants-2016_04