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Water → 2-(7-Chloro-4-quinolinylamino)-5-fluoro-benzoic acid

HRID 224587
ノート
印刷プレビュー

反応式

HRID 224587 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:12][C:13]3[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:14]=3[C:15]([O:17]C)=[O:16])=[CH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.[OH-].[Na+].O>CO>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:12][C:13]3[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:14]=3[C:15]([OH:17])=[O:16])=[CH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 23331682Methyl 2-(7-chloro-4-quinolinylamino)-5-fluoro-benzoate

生成物 1

HCID 233316862-(7-Chloro-4-quinolinylamino)-5-fluoro-benzoic acid収率 99.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1.8 g of the ester of Example 1, 25 ml of N sodium hydroxide solution, 25 ml of water and 100 ml of methanol was heated at 70°-75° C. for 90 minutes and the methanol was then evaporated. 100 ml of water and 10 ml of dimethylformamide were added to the mixture which was then heated to reflux. 4 ml of acetic acid were added thereto and the mixture was held in an ice bath for an hour and was then vacuum filtered. The recovered crystals were washed with water and dried to obtain 1.715 g of 2-(7-chloro-4-quinolinylamino)-5-fluoro-benzoic acid melting at 341°-342° C.

後処理

  1. customthe methanol was then evaporated
  2. addition100 ml of water and 10 ml of dimethylformamide were added to the mixture which
  3. temperaturewas then heated to reflux
  4. addition4 ml of acetic acid were added
  5. waitthe mixture was held in an ice bath for an hour
  6. filtrationvacuum filtered
  7. washThe recovered crystals were washed with water
  8. customdried

出典と根拠

ORDレコード
ord-688202f6158442129ddb04a5b7e6061c
出典データセット
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04233305

反応ノート

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