Dichloromethane → 3-(Trifluoromethyl)-5,6,7,8-tetrahydro-(1,2,4)triazolo(4,3-a)pyrazine

HRID 1863928Notes

Reaction equation

HRID 1863928 reaction equation
[F:1][C:2]([F:13])([F:12])[C:3]1[N:7]2[CH:8]=[CH:9][N:10]=[CH:11][C:6]2=[N:5][N:4]=1.ClCCl>[Pd].C(O)C>[F:12][C:2]([F:1])([F:13])[C:3]1[N:7]2[CH2:8][CH2:9][NH:10][CH2:11][C:6]2=[N:5][N:4]=1

Participants

5

Reactant 2

HCID 6344DichloromethaneHCID 299234623-(Trifluoromethyl)-1,2,4-triazolo(4,3-a)pyrazine

Product 1

HCID 101764893-(Trifluoromethyl)-5,6,7,8-tetrahydro-(1,2,4)triazolo(4,3-a)pyrazine

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

3-(Trifluoromethyl)-1,2,4-triazolo[4,3-a]pyrazine (540 mg, 2.87 mmol, from Step A) was hydrogenated under atmospheric hydrogen with 10% Pd/C (200 mg) as a catalyst in ethanol (10 mL) at ambient temperature for 18 h. Filtration through Celite followed by concentration gave a dark colored oil. Dichloromethane was added to the above oil and the insoluble black precipitate was filtered off. Concentration of the filtrate gave the title compound as an oil.

Workup

  1. filtrationFiltration through Celite
  2. concentrationfollowed by concentration
  3. customgave a dark colored oil
  4. filtrationthe insoluble black precipitate was filtered off

Sources & evidence

ORD record
ord-15ae0166de7c4bc0941e3f23c4d661f1
Source dataset
uspto-grants-2009_12
Patent number
US07625888B2

Reaction notes

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