Dibromomethane → 1-[Ethoxy(isothiocyanato)phosphoryl]oxyethane

HRID 462076

Reaktionsgleichung

Reaktionsgleichung von HRID 462076
[Na].[K].[S-:3][C:4]#[N:5].[NH4+].C(Br)Br.[CH2:10]([O:12][P:13](Cl)([O:15][CH2:16][CH3:17])=[O:14])[CH3:11]>C(Cl)Cl.C(Cl)(Cl)Cl.C(Cl)CCl.C1(C)C(C)=CC=CC=1.C1(C)C=CC=CC=1.C1C=CC=CC=1>[CH2:10]([O:12][P:13]([N:5]=[C:4]=[S:3])([O:15][CH2:16][CH3:17])=[O:14])[CH3:11]

Komponenten

12

Edukt 5

HCID 3024DibromomethaneHCID 13139Diethyl chlorophosphateHCID 15666Ammonium thiocyanateHCID 5360545SodiumHCID 5462222Potassium

Produkt 1

HCID 5568321-[Ethoxy(isothiocyanato)phosphoryl]oxyethane

Reagenzien, Katalysatoren, Lösungsmittel 6

HCID 111,2-DichloroethaneLösungsmittelHCID 241BenzeneLösungsmittelHCID 1140TolueneLösungsmittelHCID 6212ChloroformLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

To a stirred slurry of 1.0 to 1.1 molar equivalent of anhydrous sodium, potassium or ammonium thiocyanate in about 50 ml to 100 ml of a solvent such as benzene, toluene, xylene, ehtylene dichloride, chloroform, methylene chloride or methylene bromide, is added one molar equivalent of diethoxyphosphoryl chloride of formula (II) at a temperature range of 5° C to 30° C and, preferably, 15° C to 25° C and the reaction mixture stirred for a period of time from 4 to 4 hours to yield diethoxyphosphinyl isothiocyanate of formula (III). The reaction is slightly exothermic and such exotherm easily is controlled by either adjusting the rate of addition of said phosphoryl chloride or by using a cooling bath, or by a combination of the two.

Quellen und Nachweise

ORD-Eintrag
ord-42c5bcb7ae604546b28f0cd5d812d266
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04065466

Verknüpfte Notizen

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