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Sulfuric Acid → HCID 20451897, Verbindung

HRID 1463161
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1463161
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]#[N:10])=[CH:4][C:3]=1[NH2:11].S(=O)(=O)(O)[OH:13].[OH-].[Na+]>O>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=[O:13])[NH2:10])=[CH:4][C:3]=1[NH2:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 14891906HCID 14891906, Verbindung

Produkt 1

HCID 20451897HCID 20451897, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 1.03 g. of 1,2-diamino-4-cyanomethylbenzene (1.03 g.) was slowly added concentrated sulphuric acid (7 ml.). The mixture was heated at 90° for 90 minutes, then poured onto 50 ml. of water and ice and adjusted to pH 8 with NaOH. The precipitate which formed on cooling was discarded and the aqueous phase was concentrated to drynes. The residue was extracted with acetone, the extracts were concentrated and chromatographed on silica gel using CH2Cl2 /MeOH 9:1 to 8:2 v/v to give 1,2-diamino-4-carbamoylmethylbenzene (0.65 g.) which was used without further purification.

Aufarbeitung

  1. temperatureThe mixture was heated at 90° for 90 minutes
  2. additionpoured onto 50 ml
  3. customThe precipitate which formed
  4. temperatureon cooling
  5. concentrationthe aqueous phase was concentrated to drynes
  6. extractionThe residue was extracted with acetone
  7. concentrationthe extracts were concentrated
  8. customchromatographed on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-c3ff2f557df14504940415bd5b70f12f
Quelldatensatz
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04463173

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