HCID 13187608, compound → HCID 13187609, compound

HRID 905031Notes

Reaction equation

HRID 905031 reaction equation
Cl.Cl.[C:3]([CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][N:18]([NH:21][CH2:22][C:23]#[N:24])[CH2:17][CH2:16]1)(=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[N:25]([O-])=[O:26].[Na+]>O>[C:3]([CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][N:18]([N:21]([CH2:22][C:23]#[N:24])[N:25]=[O:26])[CH2:17][CH2:16]1)(=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

Participants

4

Reactant 2

HCID 13187608HCID 13187608, compoundHCID 23668193Sodium Nitrite

Product 1

HCID 13187609HCID 13187609, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2.0 g of 4-(4-benzoylbutyl)-1-(cyanomethylamino)-piperazine dihydrochloride was dissolved in 22 ml of water, and while the solution was cooled to below 5° C., an aqueous solution containing 1.0 g of sodium nitrite was added over the course of 10 minutes. The reaction was carried out at this temperature for 2 hours. The reaction mixture was extracted with chloroform. The extract was washed with water and dried, and the chloroform was distilled off to give 4-(4-benzoylbutyl)-1-(N-nitrosocyanomethylamino)-piperazine.

Workup

  1. temperaturewhile the solution was cooled to below 5° C.
  2. additionwas added over the course of 10 minutes
  3. extractionThe reaction mixture was extracted with chloroform
  4. washThe extract was washed with water
  5. customdried
  6. distillationthe chloroform was distilled off

Sources & evidence

ORD record
ord-6c667e01a0584ef3a5de4d54d0825ac2
Source dataset
uspto-grants-1983_12
Patent number
US04421754

Reaction notes

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