HCID 64853602, compound → HCID 55275761, compound

HRID 2239314Notes

Reaction equation

HRID 2239314 reaction equation
[F:1][C:2]1[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][C:3]=1[O:4][CH2:5][CH2:6][C:7]([OH:9])=O>O>[F:1][C:2]1[CH:13]=[CH:12][C:11]([CH3:14])=[C:10]2[C:3]=1[O:4][CH2:5][CH2:6][C:7]2=[O:9]

Participants

3

Reactant 1

HCID 64853602HCID 64853602, compound

Product 1

HCID 55275761HCID 55275761, compoundYield 102.9%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of 3-(2-fluoro-5-methylphenoxy)propanoic acid (2.45 g, 12.4 mmol, STEP 1-1) in polyphosphoric acid (35 g) was stirred at 100° C. for 2 hours. After cooling to room temperature, the mixture was diluted with water (150 mL), and extracted with ethyl acetate (60 mL×2). The organic layers were combined, washed with brine, dried over magnesium sulfate, and concentrated in vacuum to afford the title compound as a white solid (2.30 g, quant.).

Workup

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate (60 mL×2)
  3. washwashed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuum

Sources & evidence

ORD record
ord-3a8ac6d96cf44a198ebe3993e3e2b4bb
Source dataset
uspto-grants-2010_05
Patent number
US07723321B2

Reaction notes

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