HCID 22117238, compound → HCID 22117189, compound

HRID 1275899Notes

Reaction equation

HRID 1275899 reaction equation
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](O)=[O:7])=[C:4]([CH2:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Br:19])[CH:14]=2)[CH:3]=1>S1(CCCC1)(=O)=O>[Br:19][C:15]1[CH:16]=[CH:17][C:18]2[C:6](=[O:7])[C:5]3[CH:9]=[CH:10][C:2]([Br:1])=[CH:3][C:4]=3[CH2:11][CH2:12][C:13]=2[CH:14]=1

Participants

3

Reactant 1

HCID 22117238HCID 22117238, compound

Product 1

HCID 22117189HCID 22117189, compound

Reagents, catalysts & solvents 1

HCID 31347SulfolaneSolvent

Conditions

Temperature
200 °C

Procedure

A mixture of the product of step (iv) (6.1 g), polyphosphoric acid (30 ml) and sulpholane (20 ml) was heated at 200° C. for 30 minutes. The cooled mixture was partitioned between ethyl acetate and ice/water. The organic phase was dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 50% toluene in isohexane. Yield 2.71 g.

Workup

  1. customThe cooled mixture was partitioned between ethyl acetate and ice/water
  2. dry with materialThe organic phase was dried (MgSO4)
  3. customevaporated under reduced pressure
  4. customPurification
  5. washeluting with 50% toluene in isohexane

Sources & evidence

ORD record
ord-48431b09caba455292f05e889cef59e1
Source dataset
uspto-grants-2000_12
Patent number
US06162808

Reaction notes

Loading…