Reaction #41818

ord-b01d08a8a44a47019d8d36b8551d3671

Reaction equation

COC(C)(C)C
MTBE
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1
(4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl -phenyl)-methanone
Cl
HCl
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.Cl.Cl.O
crude 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
0°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Filtrationfiltered
  2. 2
    WashThe filter cake was washed with MTBE (20 mL)
  3. 3
    Otherthe solid was dried in a vacuum oven at 60° C. for 20 h

Procedure

A solution of (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl -phenyl)-methanone (2.0 g, 6.0 mmol) in absolute EtOH (20 mL) was treated with HCl(g) (0.5 g, 13.7 mmol) at room temperature. The resulting suspension was stirred for 1 h, and then MTBE (5 mL) was added. The suspension was cooled to 0° C. and filtered. The filter cake was washed with MTBE (20 mL), and the solid was dried in a vacuum oven at 60° C. for 20 h to yield crude title compound as a white solid.

Source

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