Methane → 3-(Ethylhydroxyphosphinyl)propionic acid sodium salt
Reaction equation
[CH2:1]([P:3]([CH2:6][CH2:7][CH2:8][OH:9])(=[O:5])[OH:4])[CH3:2].[OH-:10].[Na+:11].C.OO>O>[Na+:11].[CH2:1]([P:3]([OH:4])([CH2:6][CH2:7][C:8]([O-:10])=[O:9])=[O:5])[CH3:2]Participants
6
Conditions
- Temperature
- 70 °C
Procedure
15.2 g (0.1 mol) of ethyl-3-hydroxypropylphosphinic acid (produced as in Example 5) are dissolved in 150 ml of water and adjusted to pH 9 with 2N NaOH solution. Then, 0.45 g of charcoal with 5% Ft and 1% Bi is added, the suspension is heated to 70° C. and 30% strength hydrogenperoxide solution is passed into the suspension at a flow rate of 1 mol equivalent per hour while the pH of the suspension is maintained at pH=9 by adding 2N NaOH solution. After the reaction is ended, the reaction solution is filtered to remove the catalyst, the filter residue is washed and the water is distilled off in vacuo to obtain 19.3 g (93% of theory) of 3-(ethylhydroxyphosphinyl)propionic acid sodium salt (colorless solid).
Workup
- temperatureis maintained at pH=9
- filtrationthe reaction solution is filtered
- customto remove the catalyst
- washthe filter residue is washed
- distillationthe water is distilled off in vacuo
Sources & evidence
- ORD record
- ord-4e2934cea46243a69558869c949e1bc2
- Source dataset
- uspto-grants-2015_09
- Patent number
- US09139714B2
Reaction notes
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