Hydrochloric Acid → HCID 178434587, compound
Reaction equation
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]2[N:8]=C[N:6]3[C:12]([CH3:15])=[N:13][N:14]=[C:5]3[C:4]=2[CH:3]=1.[OH-].[K+].Cl>>[NH2:8][C:9]1[CH:10]=[CH:11][C:2]([Cl:1])=[CH:3][C:4]=1[C:5]1[NH:14][N:13]=[C:12]([CH3:15])[N:6]=1Participants
4
Procedure
To a flask containing 5 gms. of 9-chloro-3-methyl-1,2,4-triazolo[4,3-c]quinazoline is added 100 ml. of a 10% KOH solution and the resulting mixture heated to reflux. A gentle reflux is maintained for a period of 51/2 hours after which time the mixture is neutralized to pH 7.0 with cooling and stirring by adding dropwise a 1:1 HCl solution. The aqueous layer is washed 3 or 4 times with ethyl acetate, washed once with H2O, dried and evaporated in vacuo to dryness. The residue is recrystallized from ether to obtain 5-(2-amino-5-chlorophenyl)-3-methyl-s-triazole, m.p. 190°-195° C.
Workup
- additionTo a flask containing 5 gms
- temperatureA gentle reflux
- temperaturewith cooling
- washThe aqueous layer is washed 3 or 4 times with ethyl acetate
- washwashed once with H2O
- customdried
- customevaporated in vacuo to dryness
- customThe residue is recrystallized from ether
Sources & evidence
- ORD record
- ord-6cd1ba5be76049b99e53fd220db0b034
- Source dataset
- uspto-grants-1977_04
- Patent number
- US04020083
Reaction notes
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