Sodium Hydroxide → 2-(8-Trifluoromethyl-4-quinolinylamino)-5-fluoro-benzoic acid

HRID 224592노트

반응식

HRID 224592 반응식
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]=[CH:10][CH:9]=[C:8]2[NH:13][C:14]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:15]=1[C:16]([O:18]C)=[O:17].[OH-].[Na+]>CO>[F:26][C:2]([F:1])([F:25])[C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]=[CH:10][CH:9]=[C:8]2[NH:13][C:14]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:15]=1[C:16]([OH:18])=[O:17]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 23331699Methyl 2-(8-trifluoromethyl-4-quinolinylamino)-5-fluoro-benzoate

생성물 1

HCID 233316892-(8-Trifluoromethyl-4-quinolinylamino)-5-fluoro-benzoic acid수율 90.4%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

A mixture of 1.45 g of the product of Example 11, 4 ml of 2 N sodium hydroxide solution and 21 ml of methanol was refluxed and the methanol was evaporated. 25 ml of water were added to the mixture and the solution was filtered through asbestos. The solution was heated to 60° C. and was acidified with concentrated hydrochloric acid. The resulting suspension was cooled and filtered and the recovered precipitate was washed with water and dried to obtain 1.26 g of 2-(8-trifluoromethyl-4-quinolinylamino)-5-fluoro-benzoic acid melting at 265°±3° C.

후처리

  1. temperaturewas refluxed
  2. customthe methanol was evaporated
  3. addition25 ml of water were added to the mixture
  4. filtrationthe solution was filtered through asbestos
  5. temperatureThe resulting suspension was cooled
  6. filtrationfiltered
  7. washthe recovered precipitate was washed with water
  8. customdried

출처 및 근거

ORD 기록
ord-7606fe2189d140119282c23c395500aa
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04233305

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