Allyl Alcohol → Ethyl-3-hydroxypropylphosphinic acid

HRID 2282071ノート

反応式

HRID 2282071 の反応式
[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[CH2:6]([OH:9])[CH:7]=[CH2:8].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Na+].[Na+]>O>[CH2:1]([P:3]([CH2:8][CH2:7][CH2:6][OH:9])(=[O:5])[OH:4])[CH3:2]

参加物

5

反応物 3

HCID 7858Allyl AlcoholHCID 62655Sodium PersulfateHCID 13411864Ethylphosphonous acid

生成物 1

HCID 86656674Ethyl-3-hydroxypropylphosphinic acid収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

564 g (6 mol) of ethylphosphonous acid (produced as in Example 1) are dissolved in 860 g of water and initially charged to a 5 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. The reaction mixture is heated to 100° C. and 406 g (7 mol) of allyl alcohol and 500 g of a 5% sodium peroxodisulfate solution (1.5 mol % based on ally alcohol) is added dropwise at atmospheric pressure over 1 h. Then, the water is distilled off in vacuo, and the residue is taken up in THF and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo to leave 812 g (89% of theory) of ethyl-3-hydroxypropylphosphinic acid as oil.

後処理

  1. additioninitially charged to a 5 l five-neck flask
  2. customequipped with thermometer
  3. temperaturereflux condenser, high-performance stirrer
  4. additionis added dropwise at atmospheric pressure over 1 h
  5. distillationThen, the water is distilled off in vacuo
  6. filtrationthe insoluble salts are filtered off
  7. customThe solvent of the filtrate is removed in vacuo

出典と根拠

ORDレコード
ord-bc0a6eae70b040a7a0ac099d034d0067
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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