4-(Aminomethyl)benzonitrile hydrochloride synthesis
- Product Name:4-(Aminomethyl)benzonitrile hydrochloride
- CAS Number:15996-76-6
- Molecular formula:C8H9ClN2
- Molecular Weight:168.62
10406-25-4
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15996-76-6
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Yield:15996-76-6 99%
Reaction Conditions:
with hydrogenchloride in ethyl acetate
Steps:
1 EXAMPLE 1
In a 200 ml four-neck flask equipped with an agitator, a thermometer, a gas conduit, and a reflux condenser, p-cyanobenzylamine (10.0 g) obtained in Preparation Example 3 was dissolved in ethyl acetate (90.0 g). While the reactor was cooled in a water bath, hydrogen chloride gas was fed into the vapor phase of the reactor while stirring. Immediately after the introduction of hydrogen chloride, heat generation was confirmed, and a white solid was precipitated. After the reaction mixture was cooled to room temperature, the white solid was separated through filtration and dried in a desiccator under vacuum, thereby yielding 12.6 g of p-cyanobenzylamine hydrochloride (yield based on p-cyanobenzylamine: 99%). Through high-performance liquid chromatographic analysis of the thus-obtained p-cyanobenzylamine hydrochloride, the p-cyanobenzylamine content in the hydrochloride was found to be 77 mass %. In addition, the hydrogen chloride content in p-cyanobenzylamine hydrochloride was found to be 23 mass % through anion chromatographic analysis. The thus-obtained p-cyanobenzylamine hydrochloride has a bulk density of 0.3 g/ml.
References:
Showa Denko K.K. US6392083, 2002, B1 Location in patent:Page column 6
17201-43-3
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15996-76-6
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15996-74-4
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143090-18-0
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15996-76-6
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3034-34-2
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15996-76-6
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