Sodium Hydroxide → 1-Methyl-1,10-phenanthrolin-2(1H)-one

HRID 716552노트

반응식

HRID 716552 반응식
[I-].[CH3:2][N+:3]1[C:16]2[C:7](=[CH:8][CH:9]=[C:10]3[C:15]=2[N:14]=[CH:13][CH:12]=[CH:11]3)[CH:6]=[CH:5][CH:4]=1.[OH-:17].[Na+]>[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+]>[CH3:2][N:3]1[C:16]2[C:7](=[CH:8][CH:9]=[C:10]3[C:15]=2[N:14]=[CH:13][CH:12]=[CH:11]3)[CH:6]=[CH:5][C:4]1=[O:17]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 117716101-Methyl-1,10-phenanthrolinium iodide

생성물 1

HCID 35813871-Methyl-1,10-phenanthrolin-2(1H)-one수율 96.4%

시약·촉매·용매 1

HCID 178511488HCID 178511488, 화합물촉매

실험 절차

To a stirred aqueous solution of potassium ferricyanide (92.2 g; 280 mmol) (1.12 L), 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).

후처리

  1. customThe resulting reaction mixture
  2. customCrude crystals which precipitated out
  3. filtrationwere filtered out
  4. customdried
  5. dissolutionThe resulting crude crystals were dissolved in toluene (1.1 L)
  6. filtrationbenzene (450 mL), and insoluble matters were filtrated out
  7. customThe filtrate was evaporated under reduced pressure
  8. washthe resulting residue was washed with isopropyl ether and ethyl acetate
  9. customdried

출처 및 근거

ORD 기록
ord-fccf4c88515e4aafb5c7bc1033719594
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187690B2

반응 노트

불러오는 중…