1-Methylpiperazine → HCID 54542539, compound

HRID 1763450Notes

Reaction equation

HRID 1763450 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl[C:9]([O:11][CH2:12][C:13]([Cl:16])([Cl:15])[Cl:14])=[O:10]>C1C=CC=CC=1>[Cl:14][C:13]([Cl:16])([Cl:15])[CH2:12][O:11][C:9]([N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)=[O:10]

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 870632,2,2-Trichloroethyl chloroformate

Product 1

HCID 54542539HCID 54542539, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent2×

Procedure

N-methylpiperazine (2 g) is dissolved in 20 ml benzene and reacted with a solution of 4.5 g 2,2,2-trichloroethyl chloroformate in 20 ml benzene, with stirring and cooling in an ice bath. After stirring for 2 hours the resulting crystals are collected by vacuum filtration, washed with ether and dried under water-pump vacuum at room temperature, to give the hydrochloride of the title compound, m.p. 238°-240° C.

Workup

  1. temperaturecooling in an ice bath
  2. stirringAfter stirring for 2 hours the resulting crystals
  3. filtrationare collected by vacuum filtration
  4. washwashed with ether
  5. customdried under water-pump vacuum at room temperature

Sources & evidence

ORD record
ord-96afa801358e4fad8705c428d7d90a96
Source dataset
uspto-grants-1978_09
Patent number
US04112091

Reaction notes

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