Potassium Nitrate → 5-Bromo-6-fluoro-8-nitroquinaldine

HRID 434667

반응식

HRID 434667 반응식
[N+:1]([O-:4])([O-])=[O:2].[K+].[Br:6][C:7]1[C:16]([F:17])=[CH:15][CH:14]=[C:13]2[C:8]=1[CH:9]=[CH:10][C:11]([CH3:18])=[N:12]2>S(=O)(=O)(O)O.ClCCl>[Br:6][C:7]1[C:16]([F:17])=[CH:15][C:14]([N+:1]([O-:4])=[O:2])=[C:13]2[C:8]=1[CH:9]=[CH:10][C:11]([CH3:18])=[N:12]2

참가 물질

5

반응물 2

HCID 24434Potassium NitrateHCID 130353135-Bromo-6-fluoro-2-methylquinoline

생성물 1

HCID 131919625-Bromo-6-fluoro-8-nitroquinaldine수율 91.8%

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매2회HCID 6344Dichloromethane용매

실험 절차

A solution of 11.5 g of potassium nitrate in 30 ml of concentrated sulfuric acid was added to 21.0 g of 5-bromo-6-fluoroquinaldine in 117 ml of concentrated sulfuric acid dropwise at -5° C. After stirring at room temperature for 5 hours, the reaction mixture was poured into 2 l of ice water to precipitate solids which were then collected by filtration. The filtrate was rendered alkaline to form a small amount of solids, which together with the former solids were dissolved in dichloromethane. After the solution was dried over sodium sulfate the solvent was distilled off. Recrystallization of the residue from isopropanol gave 22.9 g of 5-bromo-6-fluoro-8-nitroquinaldine. m.p. 135°-137° C.

후처리

  1. customto precipitate solids which
  2. filtrationwere then collected by filtration
  3. customto form a small amount of solids, which together with the former solids
  4. dry with materialAfter the solution was dried over sodium sulfate the solvent
  5. distillationwas distilled off
  6. customRecrystallization of the residue from isopropanol

출처 및 근거

ORD 기록
ord-3ce4858b3b4c477693aa3864b68984a6
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04399134

연결된 노트

불러오는 중…