Phosphorus oxychloride → HCID 58976941, compound
Reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][C:12]2[N:25]=[C:15]3[NH:16][C:17](=O)[C:18]4[C:23]([N:14]3[N:13]=2)=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P(Cl)(Cl)([Cl:28])=O>>[Cl:28][C:17]1[C:18]2[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:14]2[N:13]=[C:12]([NH:11][C:5]3[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=3)[N:25]=[C:15]2[N:16]=1Participants
3
Conditions
- Temperature
- 90 °C
Procedure
A suspension of 2-(3,4-Dimethoxy-phenylamino)-4H-[1,2,4]triazolo[1,5-a]quinazolin-5-one (57 mg) in phosphorus oxychloride (5 mL) was heated at 90° C. for 2 h. Evaporation. The residue was suspended in dichloromethane, washed with cold sodium bicarbonate, brine and dried (Na2SO4). Filtration and concentration gave crude (5-Chloro-[1,2,4]triazolo[1,5-a]quinazolin-2-yl)-(3,4-dimethoxy-phenyl)-amine (68 mg). LC-MS: m/e=356.1 (M+H),
Workup
- customEvaporation
- washwashed with cold sodium bicarbonate, brine
- dry with materialdried (Na2SO4)
- filtrationFiltration and concentration
Sources & evidence
- ORD record
- ord-26fc430b6b6b489fb7d8f0e6c19366ed
- Source dataset
- uspto-grants-2007_10
- Patent number
- US07279469B2
Reaction notes
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