Potassium Iodide → 4-Fluoro-2-iodobenzoic acid

HRID 1836349노트

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HRID 1836349 반응식
N[C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].N([O-])=O.[Na+].[I-:16].[K+].S(=O)(O)[O-].[Na+]>Cl.O.S(=O)(=O)(O)O>[F:11][C:9]1[CH:8]=[CH:7][C:3]([C:4]([OH:6])=[O:5])=[C:2]([I:16])[CH:10]=1

참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 27249674-Fluoroanthranilic acidHCID 23665763Sodium BisulfiteHCID 23668193Sodium Nitrite

생성물 1

HCID 125201644-Fluoro-2-iodobenzoic acid

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 962Water용매3회HCID 1118Sulfuric Acid용매

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온도
100 °C

실험 절차

To a 0° C. mixture of 2-amino-4-fluorobenzoic acid (1.18 g, 7.6 mmol) in 12N hydrochloric acid (2.3 mL) and water (13.7 mL) was added dropwise a solution of sodium nitrite (543 mg, 7.9 mmol) in water (1.2 mL). This resulting diazonium salt solution was stirred 10 min at 0° C. A solution of potassium iodide (1.9 g) in sulfuric acid (450 35 μL) and water (3.2 mL) was added dropwise to the 0° C. solution. The reaction mixture was heated to 100° C. for 2 h then cooled to room temperature. 10% sodium bisulfite solution was added and stirred. The precipitate was filtered, washed with water, air dried and recrystallized from toluene.

후처리

  1. temperaturethen cooled to room temperature
  2. filtrationThe precipitate was filtered
  3. washwashed with water, air
  4. customdried
  5. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-fd963b0672144b37bbc2fd8b25535d54
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06777428B1

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