2-Octanone → 1-Hydroxy-1-methylheptylphosphonous acid

HRID 376053ノート

反応式

HRID 376053 の反応式
[CH3:1][C:2](=[O:9])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[OH:10][P:11]=[O:12]>CO>[OH:9][C:2]([P:11]([OH:12])[OH:10])([CH3:1])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

参加物

4

反応物 2

HCID 80932-OctanoneHCID 22497phosphenous acid

生成物 1

HCID 214699941-Hydroxy-1-methylheptylphosphonous acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of octan-2-one (3.76 g, 0.29M) and hypophosphorus acid (91.5%, 2.09 g, 0.029M) is heated at 100° C. for 12 hours in the presence of Dowex 50W x 2 ion exchange resin (1 ml, aqueous slurry). The mixture is cooled to room temperature, methanol (50 ml) is added and the Dowex is removed by filtration. The filtrate is evaporated to an oily residue, which is dissolved in ethyl acetate, washed with water, brine, then dried (MgSO4). Removal of the solvent gives 1-hydroxy-1-methylheptylphosphonous acid.

後処理

  1. customthe Dowex is removed by filtration
  2. customThe filtrate is evaporated to an oily residue, which
  3. dissolutionis dissolved in ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried (MgSO4)
  6. customRemoval of the solvent

出典と根拠

ORDレコード
ord-3033695eda954703b461a84c97d44fcc
出典データセット
uspto-grants-1996_01
特許番号
US05488171

反応ノート

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