Reaktion #328577

Reaktionsgleichung

compound ( 4 )

9-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate

sodium hydroxide

→

compound ( 3 )

2-Chloro-1.10-phenanthroline

title compound ( 5 )

9-Chloro-1-methyl-1.10-phenanthroline-2(1H)-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting reaction mixture
2. 2
   workup.STIRRINGfurther stirred at room temperature for 3.5 hours
3. 3
   SonstigeCrude crystals which precipitated out
4. 4
   Sonstigewere separated by filtration
5. 5
   Sonstigedried
6. 6
   workup.DISSOLUTIONdissolved in methanol
7. 7
   EinengenThen, a filtrate was concentrated under reduced pressure

Vorschrift

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).

Quelle