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3,4-Dichlorophenol → 2-(3,4-Dichlorophenoxy)-5-Fluoro-Benzonitrile

HRID 6898
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HRID 6898 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].C(=O)([O-])[O-].[K+].[K+].F[C:17]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:18]=1[C:19]#[N:20]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[Cl:8])[O:9][C:17]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:18]=1[C:19]#[N:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 72583,4-DichlorophenolHCID 11430Potassium CarbonateHCID 1235582,5-Difluorobenzonitrile

생성물 1

HCID 220192752-(3,4-Dichlorophenoxy)-5-Fluoro-Benzonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
105 °C

실험 절차

A flame-dried flask containing N2 inlet and magnetic stirrer was charged with 2.9 g (18 mmol) of 3,4-dichlorophenol, 6.2 g (45 mmol) of potassium carbonate and 50 mL of anhydrous DMF. With stirring, 2.08 g (15 mmol) of 2,5-difluorobenzonitrile (Aldrich Chem. Co.) was added and the mixture was heated overnight at 105° C., cooled to room temperature and partitioned between water and EtOAc. The aqueous layer was reextracted with EtOAc and the combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl. After drying with MgSO4, the solvent was removed to give the title product as a light brown oil which slowly solidified, 3.5 g.

후처리

  1. additionA flame-dried flask containing N2 inlet and magnetic stirrer
  2. temperaturecooled to room temperature
  3. custompartitioned between water and EtOAc
  4. washthe combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl
  5. dry with materialAfter drying with MgSO4
  6. customthe solvent was removed

출처 및 근거

ORD 기록
ord-46b34f726ee24169b4da1dd46149cf32
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07084165B2

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