Fumaric Acid → (4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone Mono-fumarate Salt

HRID 13539

反応式

HRID 13539 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]/[C:28]([OH:30])=[O:29]>C1COCC1>[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]/[C:28]([OH:30])=[O:29].[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:13]=[CH:14][C:15]([CH2:18][N:19]3[CH2:20][CH2:21][O:22][CH2:23][CH2:24]3)=[CH:16][CH:17]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 444972Fumaric AcidHCID 10042344(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone

生成物 1

HCID 86612815(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone Mono-fumarate Salt

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
60 °C

実験手順

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.

後処理

  1. temperatureThe resulting suspension was cooled to 0° C.
  2. filtrationthe resulting precipitate was collected by filtration
  3. washwashed with THF (20 mL)
  4. customdried in a vacuum oven at 65° C. for 20 h

出典と根拠

ORDレコード
ord-f0894e8bd35041a1ae53487d335036c1
出典データセット
uspto-grants-2010_06
特許番号
US07728129B2

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