Chloroacetyl chloride → 2-Chloro-1-(4-methylpiperazin-1-yl)ethanone
Reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Cl:8][CH2:9][C:10](Cl)=[O:11]>ClCCl>[Cl:8][CH2:9][C:10]([N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)=[O:11]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
To a solution of N-methylpiperazine (0.096 mL, 0.86 mmol, d=0.902) stirring in dichloromethane (5 mL) at 0° C., was added chloro acetylchloride (0.034 mL, 0.43 mmol, d=1.419). After stirring at 0° C. for an hour, the reaction mixture was diluted with dichloromethane (25 mL), washed with dilute citric acid, water and brine. The organic phase was dried over MgSO4, filtered and concentrated in vacuo to obtain 2-chloro-1-(4-methylpiperazin-1-yl)ethanone.
Workup
- washwashed with dilute citric acid, water and brine
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
Sources & evidence
- ORD record
- ord-ba1f1effa7b545fd91e989bda33e6774
- Source dataset
- uspto-grants-2015_10
- Patent number
- US09156840B2
Reaction notes
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