Sodium Hydroxide → 2-Chloro-1,10-phenanthroline

HRID 716555

Reaktionsgleichung

Reaktionsgleichung von HRID 716555
S([O-])(O)(=O)=O.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19]([N:20]=1)=[C:18]1[C:13]([CH:14]=[CH:15][CH:16]=[N+:17]1[CH3:21])=[CH:12][CH:11]=2.[OH-:22].[Na+]>[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+]>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19](=[C:18]3[C:13](=[CH:12][CH:11]=2)[CH:14]=[CH:15][CH:16]=[N:17]3)[N:20]=1.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[C:19]([N:20]=1)=[C:18]1[C:13]([CH:14]=[CH:15][C:16](=[O:22])[N:17]1[CH3:21])=[CH:12][CH:11]=2

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 866711149-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate

Produkt 2

HCID 3551932-Chloro-1,10-phenanthrolineHCID 28475409-Chloro-1-methyl-1,10-phenanthrolin-2(1H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 178511488HCID 178511488, VerbindungKatalysator

Versuchsvorschrift

To a stirred aqueous solution of potassium ferricyanide (22.1 g; 673 mmol) (200 mL) in an ice bath, compound (4) (6.17 g; 26.9 mmol) and an aqueous sodium hydroxide (16.14 g; 404 mmol) (110 mL) were alternately added over 20 minutes. The resulting reaction mixture was stirred in an ice bath, and further stirred at room temperature for 3.5 hours. Crude crystals which precipitated out were separated by filtration and dried, and then dissolved in methanol, and subsequently subjected to an activated carbon treatment. Then, a filtrate was concentrated under reduced pressure to give 4.26 g (yield: 72% from compound (3)) of the title compound (5).

Aufarbeitung

  1. customThe resulting reaction mixture
  2. stirringfurther stirred at room temperature for 3.5 hours
  3. customCrude crystals which precipitated out
  4. customwere separated by filtration
  5. customdried
  6. dissolutiondissolved in methanol
  7. concentrationThen, a filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c2c46337889b45a49ebe53b80fec2161
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09187690B2

Verknüpfte Notizen

Wird geladen…