Sulfuric Acid → 5-Fluoro-2-nitrobenzonitrile

HRID 618678

반응식

HRID 618678 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].[N+:10]([O-])([O-:12])=[O:11].[K+].S(=O)(=O)(O)O>C(Cl)Cl>[F:1][C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[C:4]([CH:3]=1)[C:5]#[N:6]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 678803-Fluorobenzonitrile

생성물 1

HCID 37564675-Fluoro-2-nitrobenzonitrile수율 55.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Fluorobenzonitrile (25 g) was added dropwise to a stirred mixture of potassium nitrate (21.1 g) and concentrated sulphuric acid (150 ml) which had been cooled in a mixture of salt and ice. The mixture was stirred at ambient temperature for 45 minutes. The mixture was poured onto ice (800 ml) and the precipitate was isolated. The solid so obtained was dissolved in methylene chloride, dried (MgSO4) and the solution was evaporated to give 5-fluoro-2-nitrobenzonitrile (19 g).

후처리

  1. temperaturehad been cooled in a mixture of salt and ice
  2. additionThe mixture was poured onto ice (800 ml)
  3. customthe precipitate was isolated
  4. customThe solid so obtained
  5. dry with materialdried (MgSO4)
  6. customthe solution was evaporated

출처 및 근거

ORD 기록
ord-cca974b0536343ce985ecaee00ed0664
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05955464

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