Hydrochloric Acid → HCID 20378670, Verbindung

HRID 2052108Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2052108
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[N+:14]([O-])=O)[CH:4]([C:17]([OH:19])=O)[CH2:3]1.C(=O)(O)[O-].[K+].[H][H].Cl>[Ni].C(O)C.O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]2[C:8]3[C:9]([NH:14][C:17](=[O:19])[CH:4]2[CH2:3]1)=[CH:10][CH:11]=[CH:12][CH:13]=3

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 516893Potassium BicarbonateHCID 203786594-Methyl-1-(2-nitrophenyl)piperazine-2-carboxylic acidHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 20378670HCID 20378670, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 3.5 g. (0.0135 mole) of 4-methyl-1-(o-nitrophenyl)piperazine-2-carboxylic acid, 2.5 g. (0.025 mole) of potassium bicarbonate, 110 ml. of water, 110 ml. of ethanol and 21/2 teaspoons of Raney nickel is hydrogenated in a Parr apparatus for 12 hours at an initial hydrogen pressure of 47 p.s.i. The catalyst is filtered and the filtrate is acidified with dilute hydrochloric acid. The mixture is then basified with sodium hydroxide and extracted with ethylacetate. The extract is dried and concentrated to give 2.3 g. of product. This is treated with 1 equivalent of hydrogen chloride in ethanol. After standing and cooling, filtration gives 2.4 g. of product, as the hydrochloride salt, m.p. 272°-275°. Recrystallization of the salt from ethanol-water gives 1.75 g., m.p. 284°-285° dec.

Aufarbeitung

  1. additionA mixture of 3.5 g
  2. filtrationThe catalyst is filtered
  3. extractionextracted with ethylacetate
  4. customThe extract is dried
  5. concentrationconcentrated
  6. customto give 2.3 g
  7. temperaturecooling
  8. filtrationfiltration
  9. customgives 2.4 g
  10. customRecrystallization of the salt from ethanol-water
  11. customgives 1.75 g

Quellen und Nachweise

ORD-Eintrag
ord-98e2fd1395354b6686fd8ecb1803a35a
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04182872

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