ChemicalBook CAS DataBase List Ammonium chloride

Ammonium chloride synthesis

7synthesis methods

Product Name:Ammonium chloride
CAS Number:12125-02-9
Molecular formula:ClH4N
Molecular Weight:53.49

Ammonium chloride is prepared commercially by reacting ammonia with hydrochloric acid.

Phosphoramidothioic dichloride, N-butyl-

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94317-64-3 Synthesis

94317-64-3
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12125-02-9
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Yield:94317-64-3 70%

Reaction Conditions:

with ammonia in toluene at -40 - 70;

Steps:

6.b

Into a 4-litre sulfonation flask equipped with a mechanical stirrer, a thermometer, a dosing funnel with a calcium chloride stopper and cooled to the temperature of -40 ⁰C, 300 ml of dry toluene (water content < 500 ppm) and 15 equivalents of liquid ammonia (30 mol) were poured. 2250 ml of cooled (-17 °C) NBPCl₂ solution obtained in the previous step was added at cooling and stirring by such a rate that the temperature of the reaction mixture does not rise over -18 °C. After all the NBPCl₂ toluene solution was added, cooling of the reaction mixture was ceased and the resulting suspension was stirred for 1 hour without any tempering. During another 1 hour, the suspension was warmed to the room temperature, and during one more hour, the suspension was heated to 65-70 °C. A fume hood is recommended. After 30 minutes, the suspension was heat-filtered. The filtration cake of NH₄Cl was washed with 50 ml of hot toluene (70 ⁰C). The combined toluene filtrates were cooled to 3-5 °C, the resulting product suspension was stirred for 3 hours and then filtered. The filtration cake of the product was washed with 50 ml of cold toluene (3- 5⁰C), thoroughly sucked, dried, weighed and analysed. 234.0 g of white crystalline product NBPT (70 % of the calculated yield) was obtained, with the purity of 97.0 % (HPLC). A purity of NBPT greater than 99.0 % was achieved by simple re- crystallization from toluene.

References:

WO2010/45895,2010,A2 Location in patent:Page/Page column 11