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Potassium Hydroxide → Bis [4-[(ethoxy)(propylthio)phosphoryloxy]phenyl]sulfide

HRID 1461978
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Reaktionsgleichung

Reaktionsgleichung von HRID 1461978
[S:1]([C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[P:16](=[O:25])(Cl)([S:20][CH2:21][CH2:22][CH3:23])[O:17][CH2:18][CH3:19].[OH-:26].[K+].C1CC2OCCOCCOC3C(OCCO[CH2:51][CH2:52][O:53]C2CC1)CCCC3>C(#N)C>[CH2:18]([O:17][P:16]([O:8][C:5]1[CH:6]=[CH:7][C:2]([S:1][C:9]2[CH:14]=[CH:13][C:12]([O:15][P:16]([O:53][CH2:52][CH3:51])([S:20][CH2:21][CH2:22][CH3:23])=[O:26])=[CH:11][CH:10]=2)=[CH:3][CH:4]=1)([S:20][CH2:21][CH2:22][CH3:23])=[O:25])[CH3:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 14797Potassium HydroxideHCID 175704,4'-ThiodiphenolHCID 85955Dicyclohexano-18-crown-6HCID 11745722O-Ethyl S-propyl chlorothiophosphate

Produkt 1

HCID 13343963Bis [4-[(ethoxy)(propylthio)phosphoryloxy]phenyl]sulfide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342
Acetonitrile
Lösungsmittel

Versuchsvorschrift

To a 250 ml round bottom flask was added 4,4'-thiodiphenol (4.36 g, 20 mmol), O-ethyl S-n-propyl phosphorochloridothioate (9.12 g, 45 mmol), powdered potassium hydroxide (3.37 g, 60 mmol), dicyclohexano-18-crown-6 (catalytic quantity), and acetonitrile. This mixture was refluxed 14 hours, cooled to room temperature, and the organic soluble fraction decanted from the solids. The organic solution was diluted with ether and successively washed with 4M NaOH (3×100 ml), water (2×50 ml), 5% HCl (1×50 ml), water (2×50 ml), and brine (2×50 ml). After drying (MgSO4) the solution was concentrated under reduced pressure to give a colorless oil (4.8 g, 7.6 mmol).

Aufarbeitung

  1. temperatureThis mixture was refluxed 14 hours
  2. customthe organic soluble fraction decanted from the solids
  3. additionThe organic solution was diluted with ether
  4. washsuccessively washed with 4M NaOH (3×100 ml), water (2×50 ml), 5% HCl (1×50 ml), water (2×50 ml), and brine (2×50 ml)
  5. dry with materialAfter drying (MgSO4) the solution
  6. concentrationwas concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-fc5b32dd410548f1b4fb89eab4fa1bc5
Quelldatensatz
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04457922

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