HCID 13999247, Verbindung → 2-Ethyl-2-methylbutyric acid

HRID 1165110

Reaktionsgleichung

Reaktionsgleichung von HRID 1165110
[CH2:1]([C:3]([CH3:19])([CH2:17][CH3:18])[C:4](=[O:16])CC(N)(P(O)(=O)O)P(O)(=O)O)[CH3:2].N([O-])=[O:21].[Na+]>O>[CH2:17]([C:3]([CH3:19])([CH2:1][CH3:2])[C:4]([OH:16])=[O:21])[CH3:18]

Komponenten

4

Edukt 2

HCID 13999247HCID 13999247, VerbindungHCID 23668193Sodium Nitrite

Produkt 1

HCID 298462-Ethyl-2-methylbutyric acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

0.20 mol (63.4 g) 4-ethyl-4-methyl-3-oxo-1-aminohexane-1,1-di-phosphonic acid (IV) R2 =R3 =CH2CH3, R4 =CH3) were suspended in 600 ml 2N hydrochloric acidd and a solution of 0.8 mol (55.2 g) sodium nitrite dissolved in 1104 ml water were added dropwise to the resulting suspension with stirring over a period of 7 hours at 50° C. 2-Ethyl-2-methyl-butyric acid was formed as the organic phase and was extracted with ether. Unused nitrous acid was removed with hydrazine before working up. The aqueous phase was concentrated to around 300 ml in a rotary evaporator and alkylized to pH 9 with sodium hydroxide. The tetrasodium salt of hydroxyacetonitrile diphosphonic acid (III, M=Na) crystallized out from the cold solution in the form of the octahydrate. The yield comprised 65% (58.4 g).

Aufarbeitung

  1. additionwere added dropwise to the resulting suspension

Quellen und Nachweise

ORD-Eintrag
ord-3789f7b1958042fbb2412a0d9ee6956a
Quelldatensatz
uspto-grants-1990_03
Patentnummer
US04908138

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