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ChemicalBook CAS DataBase List 1-(3-Chlorophenyl)-4-(3-chloropropyl)piperazine hydrochloride
52605-52-4

1-(3-Chlorophenyl)-4-(3-chloropropyl)piperazine hydrochloride synthesis

2synthesis methods
-

Yield:52605-52-4 88%

Reaction Conditions:

Stage #1:1-(3-chlorophenyl)piperazine hydrochloride;1.3-chlorobromopropane with tetrabutylammomium bromide;potassium carbonate in acetonitrile for 0.0111111 h;Microwave irradiation;
Stage #2: with hydrogenchloride in 1,4-dioxane;acetoneSolvent;

Steps:

3.6.1. Preparation of 1-(3-Chloropropyl)-4-(3-chlorophenyl)piperazine (5) under Microwave Radiation(Samsung M182DN; 300 W)
Firstly, 2.50 cm3 (26 mmol, 4.09 g) of 1-bromo-3-chloropropane (2a), 2.33 g (10 mmol) of1-(3-chlorophenyl)piperazine hydrochloride (4), 320 mg (10 mmol) of TBAB, 4.14 g (30 mmol) ofK2CO3, and 3 cm3 of acetonitrile/DMF were placed in a conical flask, after which the mixture wassubjected to microwave radiation. The progress of the reaction was monitored by TLC (eluentchloroform-methanol 9:1). After the reaction, 50 cm3 of water was added and the resulting productwas filtered o. After drying, obtained 5 was dissolved in acetone and a solution of 2M HCl in dioxanewas added until acidic (universal indicator). The precipitated hydrochloride was filtered o on aBüchner funnel; Rf = 0.83. The reaction yields are summarized in Table 3.

References:

Jaskowska, Jolanta;Zar eba, Przemys?aw;Sliwa, Pawe?;Pindelska, Edyta;Sata?a, Grzegorz;Majka, Zbigniew [Molecules,2019,vol. 24,# 8,art. no. 1609]

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