1-[2-(2,4-DiMethylphenylsulfanyl)phenyl]piperazine Hydrochloride synthesis

10synthesis methods

Product Name:1-[2-(2,4-DiMethylphenylsulfanyl)phenyl]piperazine Hydrochloride
CAS Number:960203-28-5
Molecular formula:C18H23ClN2S
Molecular Weight:334.9066

508233-74-7 Synthesis

508233-74-7
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1-[2-(2,4-DiMethylphenylsulfanyl)phenyl]piperazine Hydrochloride

960203-28-5
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Yield:960203-28-5 99%

Reaction Conditions:

with hydrogenchloride in diethyl ether;ethyl acetate at 30; pH=1 - 2; for 1 h;Product distribution / selectivity;

Steps:

5a

Example 5 a; Preparation of hydrochloride salt of compound I; 1.0 gram of l-[2-(2,4-Dimethylphenylsulfanyl)-phenyl]piperazine oil was dissolved in 20 ml ethyl acetate using gentle heating (30 ⁰C). When a clear solution was obtained a solution of 2 M HCl in diethyl ether was added slowly until pH was approximately 1-2. During the addition spontaneous precipitation was observed. After final addition the suspension was stirred for 1 hour before the white precipitate was isolated by filtration and dried in vacuum (40 ⁰C) overnight. l-[2-(2,4-Dimethylphenylsulfanyl)- phenyljpiperazine hydrochloride was isolated in 1.1 gram (99 %). NMR complies with structure. Elemental analysis: 64.18%C, 8.25%N, 6.96%H (Theory for 1:1 salt when corrected for 0.66% of water as determined by TGA: 64.13%C, 8.31%N, 6.95%H);Example 5b; Characterisation of the hydrochloride of compound I; The hydrochloride, as prepared in example 5 a, is crystalline (XRPD) - see Figure 7. It has a melting point of ~236°C. It absorbs about 1.5% of water when exposed to high relative humidity and has a solubility of 3 mg/ml in water.

References:

WO2007/144005,2007,A1 Location in patent:Page/Page column 31-32

960203-42-3 Synthesis