反応 #710517

ord-7d5e3737b66b411987ee8d6de9c0410f

反応方程式

CCNCC
diethylamine
CCC[NH+](CCC)CCC
tripropylammonium
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 dithiocarbamateis 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: US09302274B2uspto-grants-2016_04