Methane → 3-(Ethylhydroxyphosphinyl)propionic acid sodium salt

HRID 2282075ノート

反応式

HRID 2282075 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>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

5

反応物 3

HCID 297MethaneHCID 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% Pt and 1% Bi is added, the suspension is heated to 70° C. and air is passed through the suspension at 10 l/h. All the while, the pH of the suspension is maintained at pH=9 by adding 2N NaOH in 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 19.5 g (93% of theory) of 3-(ethylhydroxyphosphinyl)propionic acid sodium salt as colorless solid.

後処理

  1. temperatureAll the while, the pH of the suspension is 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-18c904636c53462ca28f2beb6542408a
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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