Phosphorus oxychloride → 1027775-18-3

HRID 406478Notes

Reaction equation

HRID 406478 reaction equation
[Cl:1][C:2]1[C:11]([Cl:12])=[C:10]2[C:5]([C:6](=O)[NH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:6]1[C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[N:9]=[CH:8][N:7]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 13597190617395-39-0

Product 1

HCID 866217221027775-18-3Yield 82%

Procedure

A mixture of 7,8-dichloro-3H-quinazolin-4-one (0.72 g, 3.35 mmol) in phosphorus oxychloride (6.6 g, 12.8 mmol) was heated at reflux for about 4 hours. The reaction mixture was cooled at ambient temperature then added dropwise to ice-cold water. The precipitate was collected by filtration and dried in vacuo to give 4,7,8-trichloroquinazoline as a brown solid (0.64 g, 2.74 mmol, 82%).

Workup

  1. temperaturewas heated
  2. temperatureat reflux for about 4 hours
  3. additionthen added dropwise to ice-cold water
  4. filtrationThe precipitate was collected by filtration
  5. customdried in vacuo

Sources & evidence

ORD record
ord-b0a5f99e46224dddaf8a0f6b8bb35caa
Source dataset
uspto-grants-2014_06
Patent number
US08754107B2

Reaction notes

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