HCID 22117225, compound → HCID 22117207, compound

HRID 1275912Notes

Reaction equation

HRID 1275912 reaction equation
[CH2:1]([C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][C:11]2[CH:19]=[C:18]([CH3:20])[CH:17]=[CH:16][C:12]=2[C:13]([OH:15])=O)[CH:6]=[CH:7][CH:8]=1)[CH3:2]>S1(CCCC1)(=O)=O>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]2[C:13](=[O:15])[C:12]3[CH:16]=[CH:17][C:18]([CH3:20])=[CH:19][C:11]=3[CH2:10][CH2:9][C:5]=2[CH:4]=1)[CH3:2]

Participants

3

Reactant 1

HCID 22117225HCID 22117225, compound

Product 1

HCID 22117207HCID 22117207, compound

Reagents, catalysts & solvents 1

HCID 31347SulfolaneSolvent

Conditions

Temperature
130 °C

Procedure

A mixture of the product from step (iv) in polyphosphoric acid (40 g) and sulpholane (20 ml) was heated at 130° C. for 5 hours and partitioned between ethyl acetate and water. The organic phase was washed with aqueous sodium bicarbonate and water, dried (MgSO4) and evaporated. Purified by chromatography eluting with 5% ethyl acetate inisohexane.

Workup

  1. custompartitioned between ethyl acetate and water
  2. washThe organic phase was washed with aqueous sodium bicarbonate and water
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customPurified by chromatography
  6. washeluting with 5% ethyl acetate inisohexane

Sources & evidence

ORD record
ord-7963f08ba0e846f89e5db0278258bfed
Source dataset
uspto-grants-2000_12
Patent number
US06162808

Reaction notes

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