116174-33-5 → 857995-47-2

HRID 985776Notes

Reaction equation

HRID 985776 reaction equation
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O)=[CH:5][CH:4]=1>O>[CH3:1][S:2][C:3]1[CH:4]=[C:5]2[C:6]([CH2:9][CH2:10][CH2:11][C:12]2=[O:14])=[CH:7][CH:8]=1

Participants

3

Reagents, catalysts & solvents 1

Conditions

Temperature
60 °C

Procedure

0.055 mol of the compound obtained in Step B and 100 g of polyphosphoric acid are introduced into a 500 ml round-bottomed flask. The reaction mixture is heated at 60° C. for 3 hours and is then cooled and poured into water. Extraction with ethyl ether is carried out; the organic phase is washed with water, dried over MgSO4 and evaporated under reduced pressure. The residue obtained is purified by chromatography on silica gel. Yellow oil

Workup

  1. temperatureis then cooled
  2. extractionExtraction with ethyl ether
  3. washthe organic phase is washed with water
  4. dry with materialdried over MgSO4
  5. customevaporated under reduced pressure
  6. customThe residue obtained
  7. customis purified by chromatography on silica gel

Sources & evidence

ORD record
ord-70469e88b92c4351b6b7e9591a0df28d
Source dataset
uspto-grants-2005_03
Patent number
US06872851B1

Reaction notes

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