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Methanol → HCID 67244427, Verbindung

HRID 2423338
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2423338
[NH2:1][C:2]1[C:9]([I:10])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1Cl.[CH3:12]O>C1COCC1>[NH2:7][CH2:6][C:5]1[CH:4]=[C:3]([CH3:12])[C:2]([NH2:1])=[C:9]([I:10])[CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 887MethanolHCID 26598361HCID 26598361, Verbindung

Produkt 1

HCID 67244427HCID 67244427, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

4-Amino-3-chloro-5-iodobenzonitrile (65.2 mg, 0.23 mmol) was dissolved in THF at 0° C. After Borane-THF complex (4 eq, 0.94 mmol, 0.94 ml) was slowly added into the reaction mixture. The reaction temperature was heated to reflux. The reaction mixture was stirred for 12 hrs with reflux. After confirming the completion of the reaction, MeOH was added. The mixture was stirred for 4 hrs. The reaction solvent was removed in vacuo. A residue was extracted with Ethyl acetate, washed with H2O and brine, dried with Na2SO4 and concentrated in vacuo to yield 4-Aminomethyl-2-iodo-6-methyl-phenylamine (19.4 mg).

Aufarbeitung

  1. additionAfter Borane-THF complex (4 eq, 0.94 mmol, 0.94 ml) was slowly added into the reaction mixture
  2. temperatureThe reaction temperature was heated to reflux
  3. temperaturewith reflux
  4. additionwas added
  5. stirringThe mixture was stirred for 4 hrs
  6. customThe reaction solvent was removed in vacuo
  7. extractionA residue was extracted with Ethyl acetate
  8. washwashed with H2O and brine
  9. dry with materialdried with Na2SO4
  10. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5cd0066e2f6e41dca976b0405a1c06fd
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07960584B2

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