Triethylenethiophosphoramide synthesis

Yield:52-24-4 90.7%

Reaction Conditions:

with trichlorothiophosphine at 16.5; for 0.533333 h;Temperature;

Steps:

1; 2; 3
S1: Ethyleneimine and 870 mL of organic solvent was added to the low temperature reactor, the refrigerant interlayer was turned on to pass the cold, circulation cooling, when the temperature in the reactor drops to 16.5 ° C, the stirring paddle was turned on;S2: The Thiophosphoryl chloride dissolved in an organic solvent 1690mL, and was added drop wise to the reaction kettle, when thiophosphoryl chloride organic solvent was added dropwise to 828.1 mL, the predetermined amount of thiophosphoryl chloride was added= =0 =0.49 mol / 1 mol = 49%, the acid binding agent is added drop wise, the dropping rate of the acid binding agent was 3.06 times of the dropping rate of the organic solvent thiophosphoryl chloride, and the reaction temperature was maintained at 16.5 ° C for 32 min;S3: Filtered, the filtrate solvent was evaporated under reduced pressure to obtain an organic residue , the residue was dissolved in ethyl acetate, Cyclohexane was added under stirring, stirring was continued, the solution was passed at -7 ° C, crystallized, suction filtered, and dried to obtain 171.5 g of thiotepa, yield was 90.7%, the purity was 99.3%, and the solid-liquid ratio of the residue and ethyl acetate was 1 g: 11 mL, the volume ratio of ethyl acetate to cyclohexane was 11:18.5.

References:

Heilongjiang Fuhe Pharmaceutical Group Co., Ltd.;Wu Guangyan CN108484669, 2018, A Location in patent:Paragraph 0031; 0034-0036; 0037; 0040-0042; 0043; 0046-0048

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