HCID 21470327, compound → HCID 21846840, compound

HRID 1938835Notes

Reaction equation

HRID 1938835 reaction equation
[CH3:1][P:2]([CH2:5][CH:6]([CH2:11][C:12]([O:14]C)=[O:13])[C:7]([O:9]C)=[O:8])([CH3:4])=[O:3]>O>[CH3:1][P:2]([CH2:5][CH:6]([CH2:11][C:12]([OH:14])=[O:13])[C:7]([OH:9])=[O:8])([CH3:4])=[O:3]

Participants

3

Reactant 1

HCID 21470327HCID 21470327, compound

Product 1

HCID 21846840HCID 21846840, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

80 g (0.34 mol) of dimethyl dimethylphosphinylmethylsuccinate are heated to reflux with a few drops of concentratedhydrochloric acid and 80 ml of water. Methanol slowly distils over a 70 cm silvered shell Vigreux column and at the same time a further 20 g of water are added dropwise. When the reaction is completed, the batch crystallizes. After addition of isopropanol, the mixture is stirred for several hours then filtered off by suction and dried. 65 g of dimethylphosphinylmethylsuccinic acid are obtained having a melting point of 139°-141° C. This corresponds to a yield of 92% of theory.

Workup

  1. customMethanol slowly distils over a 70 cm
  2. additionat the same time a further 20 g of water are added dropwise
  3. customthe batch crystallizes
  4. additionAfter addition of isopropanol
  5. filtrationthen filtered off by suction
  6. customdried

Sources & evidence

ORD record
ord-d8a8bb391c66449f965a53e46cb7fc97
Source dataset
uspto-grants-1997_12
Patent number
US05693842

Reaction notes

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