Carbon tetrabromide → HCID 9837766, compound

HRID 1835753Notes

Reaction equation

HRID 1835753 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

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 5 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. waitwas continued for 5 minutes at 0° C.
  4. customThe solvent was removed under reduced pressure
  5. filtrationa filter
  6. washwashed three times with ether
  7. customThe filtrate solvent was then removed under reduced pressure

Sources & evidence

ORD record
ord-7f3b57ce551642ad817ecb364fcc18b5
Source dataset
uspto-grants-2004_08
Patent number
US06774126B2

Reaction notes

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