Carbon Disulfide → 2391-78-8
Reaction equation
[CH2:1]([NH+:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2].[CH3:8][CH2:9][N:10]([C:13]([SH:15])=[S:14])[CH2:11][CH3:12].C(=S)=S.C(N(CC)CC)C.C(NCC)C>>[CH2:9]([N:10]([CH2:11][CH3:12])[C:13](=[S:14])[S-:15])[CH3:8].[CH2:1]([NH+:3]([CH2:6][CH3:7])[CH2:4][CH3:5])[CH3:2]Participants
6
Conditions
- Temperature
- 50 °C
Procedure
Preparation of triethylammonium salt of diethyl dithiocarbamate is as follows: 76 grams (1 mole) carbon disulfide and 101 grams (1 mole) triethylamine are mixed at 10° C. under nitrogen. To the mixture is added in slowly 80.5 grams (1.1 mole) diethylamine drop wise and maintain the 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.
Workup
- temperaturemaintain the temperature below 30° C
- customto remove the excess amine
- customfor the removal of low volatiles
Sources & evidence
- ORD record
- ord-7f8038ea261c479da965060a0fd43b95
- Source dataset
- uspto-grants-2016_04
- Patent number
- US09302274B2
Reaction notes
Loading…