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

HRID 2523

반응식

HRID 2523 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6520b67c10374e1083985864bd8780e4
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728835

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