Ammonia → 5-Ethyl-2,2-dimethylpiperazine

HRID 1681380Notes

Reaction equation

HRID 1681380 reaction equation
O[CH:2]([CH2:10][CH3:11])[CH2:3][NH:4][C:5]([CH3:9])([CH3:8])[CH2:6]O.[NH3:12].[H][H]>>[CH3:9][C:5]1([CH3:8])[CH2:6][NH:12][CH:2]([CH2:10][CH3:11])[CH2:3][NH:4]1

Participants

4

Reactant 3

HCID 222AmmoniaHCID 19806492HCID 19806492, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 198064915-Ethyl-2,2-dimethylpiperazineYield 70%

Procedure

In this example, another sample of 2,2-dimethyl-5-ethylpiperazine was prepared. Specifically, 150 cc of a Ni-Cu-Cr catalyst (1/8" diameter) was charged to a 0.815" ID tubular upward flow reactor. Two feeds, crude N-(2'-hydroxybutyl)-2-amino-2-methyl-1-propanol and ammonia were pumped through the catalyst bed at a rate of 0.30 lb/hr and 0.70 lb/hr, respectively. Hydrogen was also passed through the reactor at a rate of about 13 liters/hr. At 215° C. and 2200 psig, the products were collected. The resulting reaction mixture was vacuum distilled and then fractionally distilled at atmospheric pressure (b.p. 192° C.). About 70% yield of 2,2-dimethyl-5-ethylpiperazine was obtained.

Workup

  1. customAt 215° C. and 2200 psig, the products were collected
  2. customThe resulting reaction mixture
  3. distillationdistilled
  4. distillationfractionally distilled at atmospheric pressure (b.p. 192° C.)

Sources & evidence

ORD record
ord-0f7d8059281742ec96bc3d7729ed532d
Source dataset
uspto-grants-1992_12
Patent number
US05171819

Reaction notes

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