Potassium Carbonate → 1-Piperazineacetic acid, 4-methyl-, ethyl ester

HRID 352196Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 352196
Br[CH2:2][CH2:3][O:4][C:5](=[O:7])[CH3:6].C(=O)([O-])[O-].[K+].[K+].[CH3:14][N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>O1CCCC1>[CH2:3]([O:4][C:5](=[O:7])[CH2:6][N:18]1[CH2:19][CH2:20][N:15]([CH3:14])[CH2:16][CH2:17]1)[CH3:2]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 531671-Methylpiperazine

Produkt 1

HCID 2069391-Piperazineacetic acid, 4-methyl-, ethyl esterAusbeute 22 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of bromoethylacetate, 3.3 g (30.0 mmol) in 100 mL of tetrahydrofuran was added 4.14 g (30.0 mmol) of potassium carbonate and 3.3 mL (30.0 mmol) of 4-methylpiperazine. The reaction mixture stirred overnight at rt. and was concentrated to dryness. The residue was partitioned between 20% isopropanol/chloroform and saturated aqueous NaHCO3. The mixture was washed with saturated NaHCO3, washed with brine, dried over Na2SO4, filtered and concentrated to dryness to give 1.23 g (22%) of the desired product as a tan oil. MS (ion spray) 187.1 (M+).

Aufarbeitung

  1. concentrationand was concentrated to dryness
  2. customThe residue was partitioned between 20% isopropanol/chloroform and saturated aqueous NaHCO3
  3. washThe mixture was washed with saturated NaHCO3
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-77315a6e718741cfa42681667a5881c7
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06743794B2

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