Ammonium Chloride → 3-(4-Aminophenyl)isothiazolo[5,4-d]pyrimidin-4-amine

HRID 227619Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 227619
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[N:16][C:17]=3[NH2:19])[S:12][N:11]=2)=[CH:6][CH:5]=1)([O-])=O.[NH4+].[Cl-]>[Fe].C(O)C.O>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[N:16][C:17]=3[NH2:19])[S:12][N:11]=2)=[CH:6][CH:5]=1

Komponenten

5

Edukt 2

HCID 25517Ammonium ChlorideHCID 444147423-(4-Nitrophenyl)isothiazolo[5,4-d]pyrimidin-4-amine

Produkt 1

HCID 444147433-(4-Aminophenyl)isothiazolo[5,4-d]pyrimidin-4-amineAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 19096565Water ethanolLösungsmittel

Versuchsvorschrift

A mixture of Example 96F (0.95 g, 3.5 mmol), iron (0.78 g, 13.9 mmol), and NH4Cl (0.19 g, 3.5 mmol) in 9:1 ethanol/water (80 mL) was heated to 60° C. for 4 hours, cooled to room temperature, and filtered through a pad of diatomaceous earth (Celite®). The pad was washed with THF and the filtrate was concentrated. The concentrate was suspended in water and filtered. The filter cake was washed with water and dried to provide 0.82 g (97% yield) of the desired product.

Aufarbeitung

  1. filtrationfiltered through a pad of diatomaceous earth (Celite®)
  2. washThe pad was washed with THF
  3. concentrationthe filtrate was concentrated
  4. filtrationfiltered
  5. washThe filter cake was washed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a460971fa4ed47fbad10cd78486f36e4
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07560552B2

Notizen zur Reaktion

Wird geladen…