Sodium Iodide → O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate
Reaktionsgleichung
[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH3:10])[N:7]=[C:6]([CH2:11]Cl)[CH:5]=1)[CH3:2].[P:13]([O-:22])([O:19][CH2:20][CH3:21])([S:15][CH2:16][CH2:17][CH3:18])=[S:14].[K+].[I-].[Na+]>CC(C)=O>[P:13]([S:15][CH2:16][CH2:17][CH3:18])([O:19][CH2:20][CH3:21])([S:14][CH2:11][C:6]1[CH:5]=[C:4]([O:3][CH2:1][CH3:2])[N:9]=[C:8]([CH3:10])[N:7]=1)=[O:22]Komponenten
Reaktionsbedingungen
- Temperatur
- 45 °C
Versuchsvorschrift
8.0 g (0.043 mol) of 6-ethoxy-4-chloromethyl-2-methyl-pyrimidine and 10.8 g (0.045 mol) of potassium O-ethyl S-(n-propyl) dithiophosphate are suspended in 20 ml of acetone. After the addition of a small amount (spatula tip) of sodium iodide the mixture is stirred well at 45° C. for 12 hours. The mixture is then filtered through Celite, the filtrate is concentrated under reduced pressure and the thus-isolated solid is taken up in 100 ml of toluene. The toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution and dried over anhydrous sodium sulphate, and the solvent is removed by evaporation at 60° C. under reduced pressure. In this manner there is obtained O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate as an almost colourless oil, nD20 1.5385.
Aufarbeitung
- filtrationThe mixture is then filtered through Celite
- concentrationthe filtrate is concentrated under reduced pressure
- washThe toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulphate
- customthe solvent is removed by evaporation at 60° C. under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-65aaff459f064f11b28e2bf9e069b82f
- Quelldatensatz
- uspto-grants-1986_04
- Patentnummer
- US04584295
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