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Maleate(2-) → 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethylphenyl)-1-piperazineacetamide (Z)-2-butenedioate

HRID 35349
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HRID 35349 반응식
[NH2:1][C:2]([CH:4]1[N:9]([CH2:10][CH2:11][CH2:12][CH:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[CH2:8][CH2:7][N:6]([CH2:28][C:29]([NH:31][C:32]2[C:37]([CH3:38])=[CH:36][CH:35]=[CH:34][C:33]=2[CH3:39])=[O:30])[CH2:5]1)=[O:3].[C:40]([O-:47])(=[O:46])/[CH:41]=[CH:42]\[C:43]([O-:45])=[O:44]>CC(=O)C>[C:40]([OH:47])(=[O:46])/[CH:41]=[CH:42]\[C:43]([OH:45])=[O:44].[NH2:1][C:2]([CH:4]1[N:9]([CH2:10][CH2:11][CH2:12][CH:13]([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)[C:21]2[CH:22]=[CH:23][C:24]([F:27])=[CH:25][CH:26]=2)[CH2:8][CH2:7][N:6]([CH2:28][C:29]([NH:31][C:32]2[C:37]([CH3:38])=[CH:36][CH:35]=[CH:34][C:33]=2[CH3:39])=[O:30])[CH2:5]1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5288227Maleate(2-)HCID 142300883-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethylphenyl)-1-piperazineacetamide

생성물 1

HCID 867423903-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethylphenyl)-1-piperazineacetamide (Z)-2-butenedioate수율 39%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of 3 parts of 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethylphenyl)-1-piperazineacetamide in 80 parts of 2-propanone was added to a solution of 1.9 parts of (Z)-2-butenedioate in 40 parts of 2-propanone: slowly crystallization. The product was filtered off and recrystallized twice from 2-propanol and once from 2-propanone, yielding 1.56 parts (39%) of 3-(aminocarbonyl)-4-[4,4-bis(4-fluorophenyl)butyl]-N-(2,6-dimethylphenyl)-1-piperazineacetamide (Z)-2-butenedioate (1:2) monohydrate; mp. 119.6° C. (compound 174).

후처리

  1. customslowly crystallization
  2. filtrationThe product was filtered off
  3. customrecrystallized twice from 2-propanol and once from 2-propanone

출처 및 근거

ORD 기록
ord-c901156177a648379f91f3f559a43e89
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04766125

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