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ChemicalBook CAS DataBase List N-(n-Butyl)thiophosphoric triamide

N-(n-Butyl)thiophosphoric triamide synthesis

5synthesis methods
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Yield:94317-64-3 89%

Reaction Conditions:

Stage #1:N-butylamine with monothioorthophosphoric acid;dichloromethane;sodium hydroxide at 25; for 0.00555556 h;Large scale;
Stage #2: with ammonia at 15;Large scale;Temperature;

Steps:

25
In this example, 3.46 kg (2.04 mol) of thiophosphoric acid and 2.768 kg of methylene chloride were mixed, and 1.465 kg (2.0 mol) of n-butylamine was added to 2.637 kg of methylene chloride at the same time into a Corning microchannel (2.0 mol) of 10% NaOH solution was injected into the metering plunger pump, and the back pressure valve was adjusted to 0 Pa to control the speed of material entry, and the three materials were uniformly used, and the temperature Control at 25 , the reaction time is 20s.When the material enters the third plate, it is cooled to 15 , and the fourth plate is fed with NH314.96kg (8.8mol) at 15 . The material is separated by gas-liquid separation, and the inorganic layer is separated. After partial distilling off of methylene chloride, the product was cooled and crystallized, and filtered to obtain NBPT. The total yield was 89%, the product mass fraction was over 98%, and the melting point was 57.8 -58.5

References:

Zhejiang Aofutuo Chemical Co., Ltd.;Dai, Feng;Dai, jiaben;Dai, shutian;Dai, yineng CN105254664, 2016, A Location in patent:Paragraph 0062; 0063

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