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

HRID 224592ノート

反応式

HRID 224592 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7606fe2189d140119282c23c395500aa
出典データセット
uspto-grants-1980_11
特許番号
US04233305

反応ノート

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