1-Ethylpiperazine → HCID 50879465, compound
Reaction equation
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[O:11][CH3:12].[CH2:13]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[CH3:14]>O>[CH2:13]([N:15]1[CH2:20][CH2:19][N:18]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=2[O:11][CH3:12])[CH2:17][CH2:16]1)[CH3:14]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
2-Bromo-5-nitroanisole (4.7 g, 20 mmol) and N-ethyl-piperazin (10.3 ml) is stirred for 13 h at 110° C. under N2-atmosphere. Water (80 ml) is added and the mixture extracted twice with CH2Cl2 (2×80 ml). The organic phases are washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; CH2Cl2/MeOH 19:1→9:1) gives the title compound: m.p.: 84-85° C.
Workup
- extractionthe mixture extracted twice with CH2Cl2 (2×80 ml)
- washThe organic phases are washed with water and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-81044527cba54252b82d06bc6ca81839
- Source dataset
- uspto-grants-2010_01
- Patent number
- US07652022B2
Reaction notes
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