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Methane → [Hydroxy(ethyl)phosphinyl]acetic acid

HRID 1526927
ノート
印刷プレビュー

反応式

HRID 1526927 の反応式
[CH2:1]([P:3]([CH2:6][CH2:7][OH:8])(=[O:5])[OH:4])[CH3:2].[OH-:9].[Na+].C>O>[CH2:1]([P:3]([OH:4])([CH2:6][C:7]([OH:9])=[O:8])=[O:5])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 297MethaneHCID 14798Sodium Hydroxide2 回HCID 46832563HCID 46832563、化合物

生成物 1

HCID 15357685[Hydroxy(ethyl)phosphinyl]acetic acid収率 92%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

13.8 g (0.1 mol) of ethyl(2-hydroxyethyl)phosphinic acid (produced as in Example 7) 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 a rate of 10 l/h. All the while, the pH of the suspension is maintained at pH=9 by adding 2N NaOH solution. After the reaction has ended, the reaction solution is filtered to remove the catalyst, which is washed, the filtrate is made acidic with hydrochloric acid and the water is distilled off in vacuo. The residue is taken up in tetrahydrofuran and extracted. The insoluble salts are filtered off to leave 14.0 g (92% of theory) of 2-(ethylhydroxyphosphinyl)acetic acid 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, which
  4. washis washed
  5. distillationthe water is distilled off in vacuo
  6. extractionextracted
  7. filtrationThe insoluble salts are filtered off

出典と根拠

ORDレコード
ord-452e082171bf4e4489dcdfc7a20a4e5d
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09085734B2

反応ノート

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