Water → Cgp-36216

HRID 576017

反応式

HRID 576017 の反応式
[CH2:1]([P:3]([CH2:10][CH2:11][CH2:12][NH2:13])(=[O:9])[O:4]CCCC)[CH3:2].O>C(O)CCC.O>[CH2:1]([P:3]([CH2:10][CH2:11][CH2:12][NH2:13])(=[O:4])[OH:9])[CH3:2]

参加物

4

反応物 2

HCID 962WaterHCID 46212699Butyl ethyl(3-aminopropyl)phosphinate

生成物 1

HCID 9898878Cgp-36216収率 98%

試薬・触媒・溶媒 1

HCID 22253497Water butanol溶媒

実験手順

414 g (2 mol) of butyl ethyl(3-aminopropyl)phosphinate (produced as in Example 14) are initially charged to a 1 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. At 160° C., during 4 h, 500 ml of water are metered in and a butanol-water mixture is distilled off. The solid residue is recrystallized from acetone to obtain 296 g (98% of theory) of ethyl(3-aminopropyl)phosphinic acid as colorless solid.

後処理

  1. customequipped with thermometer
  2. temperaturereflux condenser, high-performance stirrer
  3. distillationis distilled off
  4. customThe solid residue is recrystallized from acetone

出典と根拠

ORDレコード
ord-56fd2f5fb68a46e3a0e6af6fcdee3663
出典データセット
uspto-grants-2015_05
特許番号
US09035088B2

関連ノート

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