반응 #41817

ord-f0894e8bd35041a1ae53487d335036c1

반응 방정식

CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1
(4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone
O=C(O)/C=C/C(=O)O
fumaric acid
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.O=C(O)/C=C/C(=O)O
crude title compound
CC(C)N1CCN(C(=O)c2ccc(CN3CCOCC3)cc2)CC1.O=C(O)/C=C/C(=O)O
(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone Mono-fumarate Salt

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The resulting suspension was cooled to 0° C.
  2. 2
    여과the resulting precipitate was collected by filtration
  3. 3
    세척washed with THF (20 mL)
  4. 4
    기타dried in a vacuum oven at 65° C. for 20 h

실험 절차

To a THF solution (40 mL) of (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone (3.0 g, 9.0 mmol) were added THF (40 mL) and fumaric acid (3.3 g, 28.4 mmol). The resulting mixture was heated to 60° C. and stirred for 0.5 h. The resulting suspension was cooled to 0° C. and the resulting precipitate was collected by filtration, washed with THF (20 mL), and dried in a vacuum oven at 65° C. for 20 h to yield crude title compound as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728129B2uspto-grants-2010_06