1-[(3,4-DIMETHOXYPHENYL)SULFONYL]PIPERAZINE synthesis
- Product Name:1-[(3,4-DIMETHOXYPHENYL)SULFONYL]PIPERAZINE
- CAS Number:91908-88-2
- Molecular formula:C12H18N2O4S
- Molecular Weight:286.35
110-85-0
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23095-31-0
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91908-88-2
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Yield:91908-88-2 65%
Reaction Conditions:
in dichloromethane;
Steps:
1.a
To a solution of 3,4-bis(methyloxy)benzenesulfonyl chloride (4 g, 16.9 mmol) in 282 mL dichloromethane (DCM), was added piperazine (2.91 g, 2 eq) all at once. The reaction appeared complete by LCMS within minutes. After stirring overnight, the reaction progress was unchanged by LCMS. The mixture was concentrated by half in vacuo. Water was added and the solution acidified by addition of 1 N hydrochloric acid (HCI). The organic layer was discarded. The aqueous layer was washed 1 x with DCM, and then made basic by addition of 1 N sodium hydroxide (NaOH). The aqueous phase was extracted with ethyl acetate (6 x 40 mL each). The combined organic phases were dried over magnesium sulfate (MgSO4), filtered, concentrated, and dried in vacuo. The final product was afforded as a white solid and 100% purity by LCMS (M+H = 287.2) and NMR (3.19 g, 65% yield). 1H NMR (DMSO-d6, 400 MHz) δ: 7.29 (1 H, dd), 7.19 (1 H, d), 7.13 (1 H, d), 3.86 (3H, s), 3.83 (3H, s), 2.76 (4H, br q), 2.70 (4H, br q).
References:
WO2007/127505,2007,A2 Location in patent:Page/Page column 39
23095-31-0
157 suppliers
$10.00/1g
91908-88-2
15 suppliers
$126.00/500mg