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6588-22-3

BUTYLPHOSPHONOTHIOIC DICHLORIDE synthesis

3synthesis methods
-

Yield:6588-22-3 95%

Reaction Conditions:

with trichlorothiophosphine;potassium carbonate in toluene at 0 - 10; for 1 h;Sonication;Time;

Steps:

1

In a 1000 ml three-necked flask, 111.8 g of thiophosphoryl chloride and 300 ml of toluene were added, and the temperature was lowered to 0-5 ° C with an ice bath.After slowly adding 45.5 g of potassium carbonate with stirring, a toluene solution of n-butylamine (50.7 g of n-butylamine, 180 ml of toluene) was added dropwise.After the addition, ultrasonic waves were applied to the reactor at a frequency of 45 KMz, and the reaction was stirred at 0-10 ° C for 1 hour.After the reaction was completely detected, toluene was recovered under reduced pressure, and the remaining material was a product, the content was 98.2%, the weight was 129 g, and the yield was 95%.

References:

CN108586523,2018,A Location in patent:Paragraph 0017; 0019; 0020; 0021; 0023; 0025