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

HRID 16419

反応式

HRID 16419 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-63c7feb226134404a5bf0269df3955a5
出典データセット
uspto-grants-2010_06
特許番号
US07737153B2

関連ノート

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