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ChemicalBook CAS DataBase List 4-Chlorophenylhydrazine hydrochloride
1073-70-7

4-Chlorophenylhydrazine hydrochloride synthesis

7synthesis methods
4-Bromochlorobenzene

106-39-8

4-Chlorophenylhydrazine hydrochloride

1073-70-7

The general procedure for the synthesis of p-chlorophenylhydrazine hydrochloride from 4-bromochlorobenzene is as follows: 98.25 g of 4-bromochlorobenzene and 3.3 equivalents of 71% hydrazine hydrate were added to a reaction vessel, to which were added 10 wt.% of the phase transfer catalyst PEG400, 3 times the weight of the solvent acrylhydrazine, and 20 wt.% of a catalyst (copper sulfate in the ratio of copper sulfate to cobalt chloride by mass of 3:1). The reaction process consisted of slowly increasing the temperature to 152 °C, refluxing or packing pressure reaction at atmospheric pressure, and maintaining the reaction at this temperature for 10 hours. During this time, the reaction process was monitored by HPLC and stopped when the amount of p-chlorophenylhydrazone no longer increased. After completion of the reaction, the solid was separated by filtration and the filtrate was distilled to remove the solvent. To the obtained residue, 30% hydrochloric acid was added, the pH was adjusted to 3, and the residue was filtered with thorough stirring. The filtrate was washed with water and dried at 55°C to finally obtain p-chlorophenylhydrazine hydrochloride. In this embodiment, the yield of p-chlorophenylhydrazine hydrochloride was 88.1% and the HPLC purity was 99.29%.

2028-74-2 Synthesis
Benzenediazonium, 4-chloro-, chloride

2028-74-2
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Yield:1073-70-7 98.2%

Reaction Conditions:

with 5% active carbon-supported ruthenium;hydrogen at 30; under 3750.38 Torr; for 4 h;Temperature;Pressure;Reagent/catalyst;

Steps:

1-4; 1-3 Example 4
A synthesis process of p-chlorophenylhydrazine hydrochloride includes the following steps:

(2) mixing substance A with a 5% ruthenium-carbon catalyst, the mass ratio of catalyst to p-chloroaniline is 0.1: 1, and nitrogen was substituted 3 times. Pass in hydrogen for 3 times and pressurize to 0.5MPa under hydrogen conditions. Heating to 30 °C, holding time 4h, filtering, it is obtained by drying at 105 °C. After testing, the yield of p-chlorophenylhydrazine hydrochloride was 98.2%, and the purity was 99.7%.

References:

CN110330443,2019,A Location in patent:Paragraph 0064-0092

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