1-(2-METHOXY-5-NITROPHENYL)PIPERAZINE synthesis
- Product Name:1-(2-METHOXY-5-NITROPHENYL)PIPERAZINE
- CAS Number:58315-37-0
- Molecular formula:C11H15N3O3
- Molecular Weight:237.26
35386-24-4
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Yield:58315-37-0 66%
Reaction Conditions:
Stage #1: 1-(2-Methoxyphenyl)piperazinewith sulfuric acid;potassium nitrate at 20; for 0.5 h;Inert atmosphere;
Stage #2: with sodium hydroxideProduct distribution / selectivity;Cooling with ice;
Steps:
9.A
Potassium nitrate (O 63 g, 6 2 mmol) was added portion-wise to a solution of 1-[2- (methyloxy)phenyl]pιperazιne (1 0 g, 5 2 mmol) in sulfuric acid (5 mL) The resulting brown solution was stirred at rt for 30 mm The reaction solution was slowly added to an ice slurry The mixture was neutralized with 5 N NaOH and extracted with EtOAc The organic fraction was washed with brine and dried over magnesium sulfate The solvent was removed under vacuum and provided 980 mg (66%) of the desired nitration product of Step A ES-LCMS m/z 238 14 (M+H)
References:
WO2010/104899,2010,A1 Location in patent:Page/Page column 126
