Piperazine → HCID 23322302, compound

HRID 1018417Notes

Reaction equation

HRID 1018417 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(C1OC1)Cl>O>[NH:1]1[CH:2]=[CH:3][N:4]=[CH:6]1.[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 7835Epichlorohydrin

Product 1

HCID 23322302HCID 23322302, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
80 °C

Procedure

68.8 g (1.0 mole) of limidazole and 260.6 g (3.0 mole) of piperazine were solved in 700.2 g of water and at a temperature of 50-60° C. 370 g (4.0 mole) of epichlorhydrin were added dropwise. After the addition was complete, the reaction mixture was stirred for additional 5 hours at 80° C. To 237 g of this product (equivalent to 1,022 mole of oxidizable nitrogen atoms) 80.7 g (1.12 mole) of a 47.2% solution of H202 in water were added over a period of 5 hours at 40° C. After that the mixture was heated to 50-60° C. until the theoretical amount of H202 had been consumed. Unreacted H202 was destroyed by using Pt/C and the solution then filtered.

Workup

  1. additionAfter the addition
  2. temperatureAfter that the mixture was heated to 50-60° C. until the theoretical amount of H202
  3. customhad been consumed
  4. customUnreacted H202 was destroyed
  5. filtrationthe solution then filtered

Sources & evidence

ORD record
ord-c8b2d32f10a54e42ba79b3e95f447033
Source dataset
uspto-grants-2002_11
Patent number
US06482787B1

Reaction notes

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