Oxalic Acid → 4-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide dioxalate

HRID 2523

反応式

HRID 2523 の反応式
[NH2:1][C@@H:2]([CH3:41])[C:3]([NH:5][CH2:6][C:7]1[CH:40]=[CH:39][C:10]([C:11]([N:13]([CH2:22][CH2:23][N:24]2[CH2:29][CH2:28][CH:27]([C:30](=[O:38])[C:31]3[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=3)[CH2:26][CH2:25]2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[O:20][CH3:21])=[O:12])=[CH:9][CH:8]=1)=[O:4].[C:42]([OH:47])(=[O:46])[C:43]([OH:45])=[O:44]>CO>[C:42]([OH:47])(=[O:46])[C:43]([OH:45])=[O:44].[C:42]([OH:47])(=[O:46])[C:43]([OH:45])=[O:44].[NH2:1][C@@H:2]([CH3:41])[C:3]([NH:5][CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:11]([N:13]([CH2:22][CH2:23][N:24]2[CH2:25][CH2:26][CH:27]([C:30](=[O:38])[C:31]3[CH:32]=[CH:33][C:34]([F:37])=[CH:35][CH:36]=3)[CH2:28][CH2:29]2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[O:20][CH3:21])=[O:12])=[CH:39][CH:40]=1)=[O:4]

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 678007174-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide

生成物 1

HCID 867522934-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide dioxalate収率 85.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide (84.7 mg, 0.155 mmol) was dissolved in methanol (5 ml) and mixed with oxalic acid (28 mg, 0.311 mmol). After 5 minutes of stirring at room temperature, methanol was removed by evaporation, and the resulting amorphous residue was washed with acetone (5 ml) and collected by filtration to obtain 84 mg (85.1%) of the title compound in a colorless amorphous powder form.

後処理

  1. custommethanol was removed by evaporation
  2. washthe resulting amorphous residue was washed with acetone (5 ml)
  3. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-6520b67c10374e1083985864bd8780e4
出典データセット
uspto-grants-1998_03
特許番号
US05728835

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