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

HRID 2371443노트

반응식

HRID 2371443 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 27249674-Fluoroanthranilic acid

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c2d1eb11bc534865acec2db3d6c493a4
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05093364

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