Water → HCID 86725102, compound
Reaction equation
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Br:8])[N:3]=1.[CH3:9][C:10]1[N:14]2[CH2:15][CH2:16][NH:17][CH2:18][C:13]2=[N:12][N:11]=1.C(=O)([O-])[O-].[K+].[K+].O>O1CCOCC1>[Br:8][C:4]1[N:3]=[C:2]([N:17]2[CH2:16][CH2:15][N:14]3[C:10]([CH3:9])=[N:11][N:12]=[C:13]3[CH2:18]2)[CH:7]=[CH:6][CH:5]=1Participants
6
Conditions
- Temperature
- 140 °C
Procedure
A glass microwave reaction vessel was charged with 2,6-dibromopyridine (434 mg, 1.832 mmol, Aldrich), 3-methyl-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazine (380 mg, 2.75 mmol, MolBridge) and potassium carbonate (253 mg, 1.832 mmol) in dioxane (1.8 mL). The reaction was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Uppsala, Sweden) at 140° C. for 4 h. The reaction was cooled to RT, H2O was added and the resulting precipitate was collected by filtration, washed with H2O and dried to give the crude product. MS (ESI, pos. ion) m/z: 294 (M+1).
Workup
- customA glass microwave reaction vessel
- temperatureThe reaction was cooled to RT
- filtrationthe resulting precipitate was collected by filtration
- washwashed with H2O
- customdried
Sources & evidence
- ORD record
- ord-a076add8fc9042eea3d9d6a4ff5230e9
- Source dataset
- uspto-grants-2016_04
- Patent number
- US09321756B2
Reaction notes
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