Phosphonic acid, P-(chloromethyl)-, diethyl ester → Diethoxyphosphinylmethylthioacetate

HRID 1646188Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1646188
[C:1]([O-:4])(=[S:3])[CH3:2].C([N+](CCCC)(CCCC)CCCC)CCC.Cl[CH2:23][P:24](=[O:31])([O:28][CH2:29][CH3:30])[O:25][CH2:26][CH3:27]>O1CCCC1>[CH2:26]([O:25][P:24]([CH2:23][O:4][C:1](=[S:3])[CH3:2])([O:28][CH2:29][CH3:30])=[O:31])[CH3:27]

Komponenten

4

Edukt 2

HCID 76633Phosphonic acid, P-(chloromethyl)-, diethyl esterHCID 178477078HCID 178477078, Verbindung

Produkt 1

HCID 53962055DiethoxyphosphinylmethylthioacetateAusbeute 70,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of tetra-n-butylammonium thioacetate (12.8 g, 0.041 mol) and diethyl chloromethylphosphonate (5 g, 0.027 mol) is stirred in tetrahydrofuran (30 ml) overnight at room temperature. After evaporation of the solvent, the residue is purified by silica gel chromatography (2:1 heptane:acetone as eluant) to give diethoxyphosphinylmethylthioacetate (4.3 g). 1H-NMR: 4H, m, 4.20-4.11 ppm; 2H, d, 3.23; 3H, s, 2.40; 6H, m, 1.33.

Aufarbeitung

  1. customAfter evaporation of the solvent
  2. customthe residue is purified by silica gel chromatography (2:1 heptane:acetone as eluant)

Quellen und Nachweise

ORD-Eintrag
ord-13e26aa07aa14c0cb045627c731bee0a
Quelldatensatz
uspto-grants-1993_01
Patentnummer
US05179085

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