Potassium Carbonate → 2-(4-Amino-2-chlorophenoxy)-6-fluorobenzonitrile

HRID 16419

반응식

HRID 16419 반응식
F[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[C:4]#[N:5].C(=O)([O-])[O-].[K+].[K+].[Cl:17][C:18]1[CH:19]=[C:20]([CH:22]=[CH:23][C:24]=1[OH:25])[NH2:21]>C(#N)C>[NH2:21][C:20]1[CH:22]=[CH:23][C:24]([O:25][C:2]2[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=2[C:4]#[N:5])=[C:18]([Cl:17])[CH:19]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 746952,6-DifluorobenzonitrileHCID 775784-Amino-2-chlorophenol

생성물 1

HCID 179793022-(4-Amino-2-chlorophenoxy)-6-fluorobenzonitrile

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1.00 g (7.19 mmol) of 2,6-difluorobenzonitrile is initially charged in 10 ml of acetonitrile. 1.99 g (14.4 mmol) of potassium carbonate and 1.03 g (7.19 mmol) of 3-chloro-4-hydroxyaniline are added, and the mixture is heated at reflux for 45 min. The mixture is filtered and the filtercake is washed with ethyl acetate and DCM. The solvent is removed under reduced pressure and the residue is by column chromatography (silica gel 60, gradient column: mobile phase: DCM:petroleum ether=2:1, then DCM).

후처리

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 45 min
  3. filtrationThe mixture is filtered
  4. washthe filtercake is washed with ethyl acetate and DCM
  5. customThe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-63c7feb226134404a5bf0269df3955a5
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737153B2

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