Phosphorus oxychloride → HCID 58926501, compound

HRID 2075702Notes

Reaction equation

HRID 2075702 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]2

Participants

4

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

  1. temperaturewith heating
  2. temperatureAfter cooling to room temperature
  3. customthe mixture was quenched with NaHCO3
  4. filtrationfiltered
  5. washThe solid material was washed with water
  6. customdried

Sources & evidence

ORD record
ord-8867071a20b1435aa99501c6ece3993b
Source dataset
uspto-grants-2011_04
Patent number
US07919621B2

Reaction notes

Loading…