Flupirtine → Flupirtine maleate

HRID 1514664노트

반응식

HRID 1514664 반응식
[CH3:1][CH2:2][O:3][C:4]([NH:6][C:7]1[CH:8]=[CH:9][C:10]([NH:14][CH2:15][C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)=[N:11][C:12]=1[NH2:13])=[O:5].[C:23]([OH:30])(=[O:29])/[CH:24]=[CH:25]\[C:26]([OH:28])=[O:27]>C(O)(C)C>[CH3:1][CH2:2][O:3][C:4]([NH:6][C:7]1[CH:8]=[CH:9][C:10]([NH:14][CH2:15][C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)=[N:11][C:12]=1[NH2:13])=[O:5].[CH:24](/[C:23]([OH:30])=[O:29])=[CH:25]/[C:26]([OH:28])=[O:27]

참가 물질

4

반응물 2

HCID 53276Flupirtine3회HCID 444266Maleic Acid2회

생성물 1

HCID 6435335Flupirtine maleate수율 99.9%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

반응 조건

온도
20 °C

실험 절차

30 g of Flupirtine base were dissolved in 1080 ml of isopropanol at 50° C. 12.8 g of Maleic acid was dissolved in 96 ml of isopropanol at 20° C. Flupirtine solution was cooled down to 20° C. Maleic acid solution was added to Flupirtine solution in the course of stirring. The sediment was formed almost at once. The mixture was heated and stirred for 60 min at 60° C. Then the mixture was cooled down to 20° C. The sediment was filtered and washed three times with cooled (0° C.) Isopropanol. The sediment formed was white. 41.4 g of the product was formed.

후처리

  1. customThe sediment was formed almost at once
  2. temperatureThe mixture was heated
  3. stirringstirred for 60 min at 60° C
  4. filtrationThe sediment was filtered
  5. washwashed three times
  6. temperaturewith cooled (0° C.) Isopropanol
  7. customThe sediment formed

출처 및 근거

ORD 기록
ord-fe41a309beb042a5bfeba9a009b3affe
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222282B2

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