Triethylamine → 4-Fluoro-2-[(1-oxopropyl)amino]benzoic acid

HRID 2371443ノート

反応式

HRID 2371443 の反応式
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[F:6][C:7]1[CH:8]=[C:9]([NH2:16])[C:10](=[CH:14][CH:15]=1)[C:11]([OH:13])=[O:12].C(N(CC)CC)C>O1CCOCC1>[F:6][C:7]1[CH:8]=[C:9]([NH:16][C:1](=[O:4])[CH2:2][CH3:3])[C:10](=[CH:14][CH:15]=1)[C:11]([OH:13])=[O:12]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 27249674-Fluoroanthranilic acid

生成物 1

HCID 167871954-Fluoro-2-[(1-oxopropyl)amino]benzoic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Propionyl chloride (1.7 ml) was added to a solution of 4-fluoroanthranilic acid (1 g) and triethylamine (2.8 ml) in 1,4-dioxane (30 ml). The mixture was heated under reflux for 4 hours, cooled and concentrated under reduced pressure. The residue was suspended in ethyl acetate and extracted with water. The organic phase was dried and evaporated and the residue purified by silica gel chromatography to give 4-fluoro-N-propionylanthranilic acid, mp 170°-171°. (Compound 9).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. extractionextracted with water
  6. customThe organic phase was dried
  7. customevaporated
  8. customthe residue purified by silica gel chromatography

出典と根拠

ORDレコード
ord-c2d1eb11bc534865acec2db3d6c493a4
出典データセット
uspto-grants-1992_03
特許番号
US05093364

反応ノート

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