Hydrochloric Acid → HCID 21532402, compound
Reaction equation
[CH2:1]([O:3][P:4]([CH2:9][CH2:10][O:11]C(=O)C)(=[S:8])[O:5][CH2:6][CH3:7])[CH3:2].Cl>CO>[CH2:1]([O:3][P:4]([CH2:9][CH2:10][OH:11])(=[S:8])[O:5][CH2:6][CH3:7])[CH3:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
149 g of 2-acetoxyethane-thiophosphonic acid-O,O-diethyl ester (preparation according to German Offenlegungsschrift No. 2.127.821) are heated to 65°-70°C in 100 ml of methanol containing 3 wt.% of HCl, while removing simultaneously by distillation a mixture of methyl acetate/methanol. The reaction is terminated after approx. 5 hours. The residue is submitted to distillation under reduced pressure; 117 g of 2-hydroxyethanethiophosphonic acid-O,O-diethyl ester (b.p. 84°-88°C/0.1 torr) are obtained, corresponding to a yield of 95% of the theoretical.
Workup
- customwhile removing simultaneously by distillation
- additiona mixture of methyl acetate/methanol
- customThe reaction is terminated after approx. 5 hours
- distillationThe residue is submitted to distillation under reduced pressure
Sources & evidence
- ORD record
- ord-27713f7210cd42efa3e22ec9df170756
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03962378
Reaction notes
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