Methane → 3-(Ethylhydroxyphosphinyl)propionic acid sodium salt

HRID 2282076ノート

反応式

HRID 2282076 の反応式
[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]

参加物

6

反応物 4

HCID 297MethaneHCID 784Hydrogen PeroxideHCID 14798Sodium Hydroxide2 回HCID 86656674Ethyl-3-hydroxypropylphosphinic acid

生成物 1

HCID 1317314203-(Ethylhydroxyphosphinyl)propionic acid sodium salt収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  1. temperatureis maintained at pH=9
  2. filtrationthe reaction solution is filtered
  3. customto remove the catalyst
  4. washthe filter residue is washed
  5. distillationthe water is distilled off in vacuo

出典と根拠

ORDレコード
ord-4e2934cea46243a69558869c949e1bc2
出典データセット
uspto-grants-2015_09
特許番号
US09139714B2

反応ノート

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