تفاعل #328577

معادلة التفاعل

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

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mixture
2. 2
   workup.STIRRINGfurther stirred at room temperature for 3.5 hours
3. 3
   أخرىCrude crystals which precipitated out
4. 4
   أخرىwere separated by filtration
5. 5
   أخرىdried
6. 6
   workup.DISSOLUTIONdissolved in methanol
7. 7
   تركيزThen, a filtrate was concentrated under reduced pressure

الإجراء التجريبي

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).

المصدر