Carbon tetrabromide → HCID 9837766, compound

HRID 2296632Notes

Reaction equation

HRID 2296632 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 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. Mass Spectra for C8H11N2O2Br: M+H=246.

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-c8b83e093f744133b86acfabf2baf22f
Source dataset
uspto-grants-2002_12
Patent number
US06489323B1

Reaction notes

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