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HCID 13355660, Verbindung → HCID 13355752, Verbindung

HRID 1111967
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1111967
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([CH:10]([OH:16])[CH2:11][NH:12][CH:13]2[CH2:15][CH2:14]2)=[CH:4][C:3]=1Br.[H][H]>CO>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH:10]([OH:16])[CH2:11][NH:12][CH:13]2[CH2:15][CH2:14]2)=[CH:6][C:7]=1[C:8]#[N:9]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 13355660HCID 13355660, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 13355752HCID 13355752, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

4 gm of 1-(4'-amino-3'-bromo-5'-cyano-phenyl)-2-cyclopropylamino-ethanol was dissolved in methanol, and the solution was hydrogenated at room temperature at a hydrogen pressure of 3 to 5 atmospheres after addition of 1 gm of palladized coal (10%). After termination of hydrogen absorption, the catalyst was suction-filtered off, the filtrate was evaporated to dryness in vacuo, and the residue was distributed between dilute sodium hydroxide and chloroform. After evaporation of the chloroform phase, 1-(4'-amino-3'-cyano-phenyl)-2-cyclopropylamino-ethanol was obtained as an oil, which was purified chromatographically on silicagel (eluant: chloroform:methanol = 9:1). The dihydrochloride, obtained by addition of ethereal hydrochloric acid, was recrystallized from isopropanol. M.p. 148°-151° C. (decomp.).

Aufarbeitung

  1. additionafter addition of 1 gm of palladized coal (10%)
  2. customAfter termination of hydrogen absorption
  3. filtrationthe catalyst was suction-filtered off
  4. customthe filtrate was evaporated to dryness in vacuo
  5. customAfter evaporation of the chloroform phase

Quellen und Nachweise

ORD-Eintrag
ord-bfe105b527cd44cf8905084057c430f1
Quelldatensatz
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04119710

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