Sodium Hydroxide → HCID 53773737、化合物

HRID 35930

反応式

HRID 35930 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[O:10][CH2:11][CH:12]([CH2:14][O:15]S(C)(=O)=O)[N:13]=1.[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:32]=[CH:31][C:30](O)=[CH:29][CH:28]=2)=[CH:23][CH:22]=1.[OH-].[Na+].[Cl-].[NH4+]>CN(C)C=O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[O:10][CH2:11][CH:12]([CH2:14][O:15][C:30]2[CH:29]=[CH:28][C:27]([C:24]3[CH:23]=[CH:22][C:21]([Cl:20])=[CH:26][CH:25]=3)=[CH:32][CH:31]=2)[N:13]=1

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 915894'-Chloro-4-biphenylolHCID 194240782-(2,6-Difluorophenyl)-4-methanesulfonyloxymethyl-2-oxazoline

生成物 1

HCID 53773737HCID 53773737、化合物収率 18.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 200 mg (0.687 mmol.) of 2-(2,6-difluorophenyl)-4-methanesulfonyloxymethyl-2-oxazoline, 232 mg (1.00 mmol.) of 4-(4-chlorophenyl)phenol, 24 mg (1.0 mmol.) of sodium hydroxide and 3 ml of N,N-dimethylformamide was stirred at room temperature for 24 hours. After the reaction was completed, the reaction mixture was poured into 50 ml of a 10% aqueous solution of ammonium chloride and extracted twice with ethyl acetate. The residue was dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 50 mg of 2-(2,6-difluorophenyl)-4-{[4-(4-chlorophenyl) phenoxy]methyl}-2-oxazoline as a white solid (m.g. 99.5° C.).

後処理

  1. extractionextracted twice with ethyl acetate
  2. dry with materialThe residue was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-20d10e61da7843ba9fa3853e27ff73ce
出典データセット
uspto-grants-1995_05
特許番号
US05411979

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