Phosphorus oxychloride → HCID 58926501, compound
Reaction equation
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[N:13][N:14]=[C:7]1[C:6](=O)[NH:5]2.P(Cl)(Cl)([Cl:24])=O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[N:13][N:14]=[C:7]1[C:6]([Cl:24])=[N:5]2Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
5z (197 mg, 0.58 mmol) was dissolved in DMF (3 mL) with heating, and then phosphorus oxychloride (0.27 mL, 2.9 mmol) was added, and the reaction was heated to 80° C. for 1.5 hours. After cooling to room temperature, the mixture was quenched with NaHCO3, and the resulting slurry was stirred at room temperature for 30 minutes and filtered. The solid material was washed with water and dried to obtain the desired product, 5aa.
Workup
- temperaturewith heating
- temperatureAfter cooling to room temperature
- customthe mixture was quenched with NaHCO3
- filtrationfiltered
- washThe solid material was washed with water
- customdried
Sources & evidence
- ORD record
- ord-8867071a20b1435aa99501c6ece3993b
- Source dataset
- uspto-grants-2011_04
- Patent number
- US07919621B2
Reaction notes
Loading…