Reaction equation
[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]Participants
12
Reactant 5
Product 1
Reagents, catalysts & solvents 6
Procedure
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.
Sources & evidence
- ORD record
- ord-42c5bcb7ae604546b28f0cd5d812d266
- Source dataset
- uspto-grants-1977_12
- Patent number
- US04065466
Linked notes
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