تفاعل #328574

معادلة التفاعل

compound ( 1 )

1-Methyl-1,10-phenanthrolinium iodide

sodium hydroxide

→

title compound ( 2 )

المردود 96.4%

1-Methyl-1,10-phenanthroline-2(1H)-one

المردود 96.4%

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mixture
2. 2
   أخرىCrude crystals which precipitated out
3. 3
   ترشيحwere filtered out
4. 4
   أخرىdried
5. 5
   workup.DISSOLUTIONThe resulting crude crystals were dissolved in toluene (1.1 L)
6. 6
   ترشيحbenzene (450 mL), and insoluble matters were filtrated out
7. 7
   أخرىThe filtrate was evaporated under reduced pressure
8. 8
   غسيلthe resulting residue was washed with isopropyl ether and ethyl acetate
9. 9
   أخرىdried

الإجراء التجريبي

To a stirred aqueous solution of potassium ferricyanide (92.2 g; 280 mmol) (1.12L), compound (1) (37.6 g; 117 mmol) and an aqueous solution of sodium hydroxide (69.3 g; 1.73 mol) (200 mL) were alternately added in an ice bath (inner temperature of 10 to 15° C.) over 20 minutes. The resulting reaction mixture was stirred at room temperature for 3 hours. Crude crystals which precipitated out were filtered out and dried. The resulting crude crystals were dissolved in toluene (1.1 L) and benzene (450 mL), and insoluble matters were filtrated out. The filtrate was evaporated under reduced pressure, and the resulting residue was washed with isopropyl ether and ethyl acetate, and then dried to give 23.7 g (yield: 75%) of the title compound (2).

المصدر