Ammonia → HCID 86630685, compound

HRID 503777Notes

Reaction equation

HRID 503777 reaction equation
[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:6](Cl)[N:5]2[N:15]=[C:16]([CH2:18][CH3:19])[N:17]=[C:4]2[N:3]=1.N>ClCCl.[Cl-].[Na+].O.[Zn]>[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][N:5]2[N:15]=[C:16]([CH2:18][CH3:19])[N:17]=[C:4]2[N:3]=1

Participants

6

Reactant 2

HCID 222AmmoniaHCID 86630686HCID 86630686, compound

Product 1

HCID 86630685HCID 86630685, compound

Reagents, catalysts & solvents 3

HCID 23994ZincCatalystHCID 6344DichloromethaneSolventHCID 57417360Sodium chloride; waterSolvent

Procedure

6.00 g 5,7-dichloro-2-ethyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine is dissolved in 180 ml dichloromethane. 180 ml saturated brine, 120 ml ammonia solution 25% w/w and 6.00 g zinc powder are added and the mixture is stirred at room temperature for 3 h. The reaction mixture is filtrated over kieselgur and is washed with dichloromethane and water. The organic phase is separated and the water phase is extracted with dichloromethane. The combined organic layers are dried over Na2SO4 and the solvent is evaporated. The residue contained 2-ethyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine. This mixture is used without further purification for the next reaction.

Workup

  1. filtrationThe reaction mixture is filtrated over kieselgur
  2. washis washed with dichloromethane and water
  3. customThe organic phase is separated
  4. extractionthe water phase is extracted with dichloromethane
  5. dry with materialThe combined organic layers are dried over Na2SO4
  6. customthe solvent is evaporated
  7. customThis mixture is used without further purification for the next reaction

Sources & evidence

ORD record
ord-47538f53fd16475e934a0024110e528b
Source dataset
uspto-grants-2010_08
Patent number
US07776864B2

Reaction notes

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