Reaktion #314399

ord-32c0b7f6220a49278e1f756d5fd51fb0

Reaktionsgleichung

COP(=S)(S)OC
dimethyl dithiophosphoric acid
CCOC(=O)/C=C\C(=O)OCC
diethyl maleate
COP(=S)(S)OC
dimethyl dithiophosphoric acid
CCOC(=O)/C=C\C(=O)OCC
diethyl maleate
Oc1ccc(O)cc1
Hydroquinone
CCOC(=O)CC(SP(=S)(OC)OC)C(=O)OCC
malathion

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeseparate solutions
  2. 2
    workup.ADDITIONan organic solution of diethyl maleate and an aqueous solution of dimethyl dithiophosphoric acid, was mixed for about 8 hours at 53° C. under a nitrogen atmosphere
  3. 3
    workup.ADDITIONAfter mixing
  4. 4
    Sonstigethe organic and aqueous solutions were separated
  5. 5
    Waschenwas washed two (2) times with water (approximately 1 liter each time)
  6. 6
    SonstigeThe organic and aqueous solutions were separated

Vorschrift

The solution of dimethyl dithiophosphoric acid was added to diethyl maleate (the ratio of dimethyl dithiophosphoric acid to diethyl maleate was approximately 1-1.25 kg: 1.2 kg). Hydroquinone (approximately 3 grams) was added to the mixture. The reaction mixture which contains two separate solutions, an organic solution of diethyl maleate and an aqueous solution of dimethyl dithiophosphoric acid, was mixed for about 8 hours at 53° C. under a nitrogen atmosphere. After mixing, the reaction was cooled to ambient temperature and the organic and aqueous solutions were separated. The organic or diethyl maleate solutions which contained malathion was washed two (2) times with water (approximately 1 liter each time). The organic and aqueous solutions were separated and the malathion in the solution of diethyl maleate retained. This reaction yielded approximately 1.5-1.9 kg of malathion.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07560445B2uspto-grants-2009_07