Phosphoric Acid → O,O-Diethyl dithiophosphate
Reaction equation
[NH4+].[CH3:2][CH2:3][O:4][P:5]([SH:10])([O:7][CH2:8][CH3:9])=[S:6].P(=O)(O)(O)O>>[CH2:3]([O:4][P:5](=[S:6])([SH:10])[O:7][CH2:8][CH3:9])[CH3:2]Participants
3
Procedure
203 g of ammonium-O,O-diethyldithiophosphate was added within 5 minutes with agitation to 485 g of 75% phosphoric acid. The reaction temperature dropped from initially 24° C down to 17° C after a post-reaction period of 10 minutes. The liquid reaction mixture was delivered to a separating vessel. It was allowed to remain therein for 10 minutes and 182.9 g of dithiophosphoric acid-O,O-diethylester was obtained as the upper phase. The yield was 98.2% of the theoretical, based on the ammonium-O,O-diethyldithiophosphate used. The product so made had a purity of 99.9% (AgNO3 and NaOH-values) (nD25 = 1.5108).
Workup
- additionThe reaction temperature dropped from initially 24° C down to 17° C
- customafter a post-reaction period of 10 minutes
- customThe liquid reaction mixture
- customwas delivered to a separating vessel
Sources & evidence
- ORD record
- ord-ea1360739aca41048598b0bf1c582ef5
- Source dataset
- uspto-grants-1977_04
- Patent number
- US04020129
Reaction notes
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