Potassium Hydroxide → HCID 23461670, compound

HRID 2286506Notes

Reaction equation

HRID 2286506 reaction equation
[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[N:9]([O-])=[O:10].[Na+].[OH-].[K+]>Cl.O>[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][N:5]([N:9]=[O:10])[CH2:4][CH2:3]1

Participants

6

Reactant 3

HCID 14797Potassium HydroxideHCID 2283491-MethylhomopiperazineHCID 23668193Sodium Nitrite

Product 1

HCID 23461670HCID 23461670, compoundYield 50%

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 962WaterSolvent

Conditions

Temperature
70 °C

Procedure

1-methylhomopiperazine (prepared as described by A. H. Sommers et al, in J. Amer. Chem. Soc. 76, 5805, 1954) (6.10 g, 0.0535 mole) was dissolved in concentrated hydrochloric acid (25 ml), cooled to 0°-5° C., stirred and treated dropwise with sodium nitrite (4.06 g) in water (10 ml). After addition the solution was allowed to come to room temperature, then heated for 1/2 hour at 70° C. The solution was cooled and basified with solid KOH and extracted with ether (3×100 ml). The dried (K2CO3) extracts yielded N-methyl-N'-nitrosohomopiperazine (3.80 g, 50%) as a pale yellow oil.

Workup

  1. temperaturecooled to 0°-5° C.
  2. additionAfter addition the solution
  3. customto come to room temperature
  4. temperatureThe solution was cooled
  5. extractionextracted with ether (3×100 ml)
  6. dry with materialThe dried (K2CO3)

Sources & evidence

ORD record
ord-759449f856244951909b77e859501755
Source dataset
uspto-grants-1981_05
Patent number
US04267175

Reaction notes

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