Water → (4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride monohydrate
Reaction equation
[ClH:1].Cl.[CH:3]([N:6]1[CH2:11][CH2:10][N:9]([C:12]([C:14]2[CH:19]=[CH:18][C:17]([CH2:20][N:21]3[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)=[CH:16][CH:15]=2)=[O:13])[CH2:8][CH2:7]1)([CH3:5])[CH3:4].O.CC(OC)(C)C>CCO>[OH2:13].[ClH:1].[ClH:1].[CH:3]([N:6]1[CH2:11][CH2:10][N:9]([C:12]([C:14]2[CH:15]=[CH:16][C:17]([CH2:20][N:21]3[CH2:22][CH2:23][O:24][CH2:25][CH2:26]3)=[CH:18][CH:19]=2)=[O:13])[CH2:8][CH2:7]1)([CH3:5])[CH3:4]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 78 °C
Procedure
A suspension of crude (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride (2.1 g, 5.2 mmol) in absolute EtOH (30 mL) was heated to 78° C. and H2O (2.2 mL) was added. The resulting solution was cooled to room temperature and MTBE (5 mL) was added. The resulting suspension was cooled to 0° C. and filtered. The filter cake was washed with MeOH (15 mL). The solids were dried in a vacuum oven at 105° C. for 20 h to yield the title compound as a white solid.
Workup
- temperatureThe resulting solution was cooled to room temperature
- temperatureThe resulting suspension was cooled to 0° C.
- filtrationfiltered
- washThe filter cake was washed with MeOH (15 mL)
- customThe solids were dried in a vacuum oven at 105° C. for 20 h
Sources & evidence
- ORD record
- ord-dc3c69c5dd1647bb86f056fed946edea
- Source dataset
- uspto-grants-2010_06
- Patent number
- US07728129B2
Reaction notes
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