Methyl iodide → HCID 15029853, compound

HRID 1534039Notes

Reaction equation

HRID 1534039 reaction equation
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[I:11])[C:7](=[O:12])[CH2:6][CH2:5]2.[C:13]([O-])([O-])=O.[K+].[K+].CI>O>[CH3:13][O:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[I:11])[C:7](=[O:12])[CH2:6][CH2:5]2

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 15029852HCID 15029852, compound

Product 1

HCID 15029853HCID 15029853, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The product of Example 60 was added to methyl ethyl ketcne (50 ml), K2CO3 (5 g) and methyl iodide (5 ml) then heated at reflux for 4 1/2 hrs. The reaction was cooled, H2O added, followed by an EtOAc extraction. The organic layer was separated, washed with brine, dried (Na2SO4), filtered and evaporated. Trituration of the residue afforded the desired compound after filtration, m.p. 129° C.-30° C.

Workup

  1. temperaturethen heated
  2. temperatureat reflux for 4 1/2 hrs
  3. temperatureThe reaction was cooled
  4. extractionfollowed by an EtOAc extraction
  5. customThe organic layer was separated
  6. washwashed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. customevaporated

Sources & evidence

ORD record
ord-e75070514acc431a9d8cea52bd2bc919
Source dataset
uspto-grants-1992_02
Patent number
US05086074

Reaction notes

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