Carbon tetrabromide → HCID 9837766, compound

HRID 1267225Notes

Reaction equation

HRID 1267225 reaction equation
O[CH2:2][CH:3]1[N:9]2[C:10](=[O:13])[O:11][N:12]=[C:8]2[CH2:7][CH2:6][CH2:5][CH2:4]1.C(Br)(Br)(Br)[Br:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[Br:15][CH2:2][CH:3]1[N:9]2[C:10](=[O:13])[O:11][N:12]=[C:8]2[CH2:7][CH2:6][CH2:5][CH2:4]1

Participants

5

Reactant 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 10154341HCID 10154341, compound

Product 1

HCID 9837766HCID 9837766, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of the product of Example 5 in dichloromethane was added carbon tetrabromide (460 mg, 1.3 mmol). This solution was cooled in an ice bath and stirred for minutes. Triphenylphosphine (437 mg, 1.6 mmol) was added to the solution and stirring was continued for 5 minutes at 0° C. before allowing it to warm slowly to room temperature. The solvent was removed under reduced pressure. The residue was placed on a filter and washed three times with ether. The filtrate solvent was then removed under reduced pressure to yield the title compound.

Workup

  1. temperatureThis solution was cooled in an ice bath
  2. stirringstirring
  3. customThe solvent was removed under reduced pressure
  4. filtrationa filter
  5. washwashed three times with ether
  6. customThe filtrate solvent was then removed under reduced pressure

Sources & evidence

ORD record
ord-90fc28e0874e49809fac2ec2196bf1c8
Source dataset
uspto-grants-2003_04
Patent number
US06552052B2

Reaction notes

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