Reaction #41819

ord-dc3c69c5dd1647bb86f056fed946edea

Reaction equation

CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.Cl.Cl
(4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride
O
H2O
COC(C)(C)C
MTBE
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.Cl.Cl.O
title compound
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.Cl.Cl.O
(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride monohydrate

Solvents

Conditions

Temperature
78°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    TemperatureThe resulting solution was cooled to room temperature
  2. 2
    TemperatureThe resulting suspension was cooled to 0° C.
  3. 3
    Filtrationfiltered
  4. 4
    WashThe filter cake was washed with MeOH (15 mL)
  5. 5
    OtherThe solids were dried in a vacuum oven at 105° C. for 20 h

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728129B2uspto-grants-2010_06