Carbon tetrabromide → HCID 9837766, compound
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]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
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
- temperatureThis solution was cooled in an ice bath
- stirringstirring
- waitwas continued for 5 minutes at 0° C.
- customThe solvent was removed under reduced pressure
- filtrationa filter
- washwashed three times with ether
- 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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