video tutorial Ammonium methylsulfate preparation from sulfamic acid

Name: video tutorial - Ammonium methylsulfate preparation from sulfamic acid
Uploaded: 2025-12-11T09:03:44.251Z
Duration: 10 min 14 s
Description: to take to either dissolve the sulfamic acid or to drive the reaction to a considerable...This goes into the flask with the sulfamic acid.

Objective: synthesize ammonium methyl sulfate from sulfamic acid and methanol via reflux; use the product in subsequent sulfamic acid reactions.
Setup: 125 g sulfamic acid crystals in a dry 500 ml flask; initial 75 ml dry methyl added; reflux with a condenser and a drying tube containing anhydrous calcium chloride (to combat hygroscopic moisture).
Process: dissolution of sulfamic acid was slow; after adding more methanol (total 225 ml) and extended reflux, the reaction progressed and more sulfamic acid dissolved.
Workup: after boiling, the mixture was cooled and subjected to distillation to remove excess methanol; initially collected ~115–145 ml methanol; process halted when temperature reached around 180°C to avoid decomposition; the mixture later solidified around 100°C as solvent was removed.
Product isolation: yielded 157 g of crude ammonium methyl sulfate as a dry white solid; potential purity ~85–90% (max theoretical yield ~94%), with some residual methyl sulfate and sulfamic acid.
Properties and tests: product dissolves readily in water (easier than sulfamic acid); pH of product solution remained acidic, suggesting remaining sulfamic acid; calcium chloride test showed no sulfate (methyl sulfate is not sulfate); reaction with NaOH and indicator paper produced an alkaline result with ammonia odor, indicating ammonium salt presence.
Crystallization: solid crystallized rapidly upon cooling and pouring onto foil; additional crystals formed inside the flask during cooling.
Conclusion: the synthesis is feasible but slow and requires patience; the product is suitable for use in subsequent experiments, despite minor impurities.