StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Acetic Acid → 2-(beta-Diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene dihydrochloride

HRID 2291446
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2291446
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][CH2:10][N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])[C:5]([N+:16]([O-:18])=[O:17])=[C:4]([NH:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH:3]=1.C(O)(=O)C.C(O)=O.[ClH:34]>C(N(CC)CC)C.O.C(O)C.[Pd]>[ClH:1].[ClH:34].[CH2:14]([N:11]([CH2:12][CH3:13])[CH2:10][CH2:9][NH:8][C:6]1[CH:7]=[CH:2][CH:3]=[C:4]([NH:19][CH2:20][CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[C:5]=1[N+:16]([O-:18])=[O:17])[CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 176Acetic AcidHCID 284Formic AcidHCID 313Hydrochloric AcidHCID 200710864-Chloro-2-(beta-diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene

Produkt 1

HCID 200710842-(beta-Diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 23938PalladiumKatalysator
HCID 702EthanolLösungsmittel
HCID 962WaterLösungsmittel
HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

300 mg of palladium at a concentration of 10% on calcium carbonate are added to 0.015 mole (5.8 g) of 4-chloro-2-(β-diethylaminoethyl)amino-6-(β-diethylaminoethyl)aminonitrobenzene in 11.1 ml of triethylamine, after which 2.86 ml of acetic acid and 2.1 ml of formic acid are added dropwise. After the end of the additions, the materials are heated under reflux for 3 hours 30 minutes. The reaction mixture is diluted with 10 ml of water. The catalyst is removed by hot filtration. The filtrate is evaporated to dryness under vacuum. The inorganic salts are precipitated by adding acetone and are removed by filtration. After evaporation of the acetone, an oil is obtained and this, after treatment with a solution of hydrochloric acid in absolute ethanol, leads to the expected product which is isolated by evaporating off the alcohol and precipitating with ethyl ether.

Aufarbeitung

  1. temperatureAfter the end of the additions, the materials are heated
  2. temperatureunder reflux for 3 hours 30 minutes
  3. customThe catalyst is removed by hot filtration
  4. customThe filtrate is evaporated to dryness under vacuum
  5. customThe inorganic salts are precipitated
  6. additionby adding acetone
  7. customare removed by filtration
  8. customAfter evaporation of the acetone
  9. customan oil is obtained

Quellen und Nachweise

ORD-Eintrag
ord-750619d960624c46842dfbc1c395a29c
Quelldatensatz
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04797129

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion