Hydrazine hydrate (1:1) → HCID 67531602, compound

HRID 1888995Notes

Reaction equation

HRID 1888995 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:15][C:14](OCC)=[N:13][CH2:12][CH2:11]1)=[O:9].O.[NH2:20][NH2:21]>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([N:10]1[CH2:11][CH2:12][NH:13][CH:14]([NH:20][NH2:21])[CH2:15]1)=[O:9]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 67531099HCID 67531099, compound

Product 1

HCID 67531602HCID 67531602, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Conditions

Temperature
25 °C

Procedure

1-[(2-chlorophenyl)carbonyl]-5-(ethyloxy)-1,2,3,6-tetrahydropyrazine (I39) (0.755 g, 2.83 mmol) dissolved in Dichloromethane (DCM) (10 mL) was added to hydrazine hydrate (0.220 mL, 7.08 mmol, commercially available from e.g. Alfa Aesar, Acros or Fluka) dissolved in Dichloromethane (DCM) (5 mL) and stirred at 25° C. for 4 hr. The solvents were removed in vacuo and the residue azeotroped with toluene (3×25 mL), to afford product in 715 mg that was used in the subsequent step without further purification.

Workup

  1. customThe solvents were removed in vacuo
  2. customthe residue azeotroped with toluene (3×25 mL)
  3. customto afford product in 715 mg that
  4. customwas used in the subsequent step without further purification

Sources & evidence

ORD record
ord-b2dfdb2b77264e42b504837882d3eef6
Source dataset
uspto-grants-2013_08
Patent number
US08501946B2

Reaction notes

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