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Water → HCID 86725102, compound

HRID 634160
Notes
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Reaction equation

HRID 634160 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]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 122742,6-DibromopyridineHCID 516065053-Methyl-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine

Product 1

HCID 86725102HCID 86725102, compound

Reagents, catalysts & solvents 1

HCID 312751,4-Dioxane
Solvent

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

  1. customA glass microwave reaction vessel
  2. temperatureThe reaction was cooled to RT
  3. filtrationthe resulting precipitate was collected by filtration
  4. washwashed with H2O
  5. customdried

Sources & evidence

ORD record
ord-a076add8fc9042eea3d9d6a4ff5230e9
Source dataset
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09321756B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes