Hydrogen Sulfide → Diisobutyl phosphorodithioate
Reaction equation
[CH3:1][CH:2]([CH3:5])[CH2:3][OH:4].[P:6]12([S:18]P3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:7].S>>[CH3:1][CH:2]([CH3:5])[CH2:3][O:4][P:6]([SH:18])(=[S:7])[O:4][CH2:3][CH:2]([CH3:5])[CH3:1]Participants
Conditions
- Temperature
- 60 °C
Procedure
Into a four-necked flask equipped with a stirrer, condenser, dropping funnel and thermometer were added 608 g (8.2 moles) of 2-methyl-1-propanol and the contents were heated to 60° C. At that temperature, 444.5 g (2.0 mole) of phosphorus pentasulfide was added portion-wise over a 3-hour period with agitation. After all of the sulfide reactant was introduced, the temperature was raised to 65° C. and held for 3 hours. The evolution of hydrogen sulfide gas was trapped by a caustic scrubber which indicates a substantially complete reaction. The reaction was then allowed to cool to ambient temperature under a nitrogen blanket and the solution was filtered through diatomaceous earth to produce a greenish fluid (927 g) as the desired phosphorodithioic acid.
Workup
- customInto a four-necked flask equipped with a stirrer, condenser
- temperaturethe temperature was raised to 65° C.
- customa substantially complete reaction
- temperatureto cool to ambient temperature under a nitrogen blanket
- filtrationthe solution was filtered through diatomaceous earth
Sources & evidence
- ORD record
- ord-5bbf49e56c09452eb1d6a165e4e4f3ea
- Source dataset
- uspto-grants-1995_08
- Patent number
- US05437694
Reaction notes
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