Water → 3-(Hydroxyphenylphosphinyl)propanoic acid

HRID 726832ノート

反応式

HRID 726832 の反応式
Cl[P:2](Cl)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:10]([O:18]OC(C)(C)C)(=[O:17])[C:11]1C=CC=C[CH:12]=1.C(O)(=[O:27])C=C.[OH2:29]>>[OH:29][P:2]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)([CH2:12][CH2:11][C:10]([OH:18])=[O:17])=[O:27]

参加物

5

反応物 4

HCID 962WaterHCID 6581Acrylic AcidHCID 11966tert-Butyl peroxybenzoateHCID 12573Phenyl phosphorus dichloride

生成物 1

HCID 112873403-(Hydroxyphenylphosphinyl)propanoic acid

実験手順

Using 501.2 g of dichlorophenylphosphine, 3.2 g of t-butyl peroxybenzoate, 201.8 g of acrylic acid, and 0.92 L of water, a rinse-purified 3-[hydroxy(phenyl)phosphinyl]propionic acid was prepared by the procedure described in U.S. Pat. No. 5,334,760, namely the steps of hydrolyzing the reaction mixture after completion of the reaction, cooling it, harvesting the resulting crystals by filtration, rinsing the crystal crop with water, and drying it. The yield was 564.9 g or 94.2%. From the area ratio of the respective signals on the 1H-NMR spectrum, the molar ratio of 3-[hydroxy(phenyl)phosphinyl]propionic acid to phenylphosphinic acid was found to be 99.10:0.9. The other components were traces below the detection limit.

後処理

  1. customafter completion of the reaction
  2. temperaturecooling it
  3. filtrationby filtration
  4. washrinsing the crystal crop with water
  5. customdrying it

出典と根拠

ORDレコード
ord-672c6a8627e747fd89bac10dea930674
出典データセット
uspto-grants-1998_01
特許番号
US05710308

反応ノート

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