Pyridine → (3,5-Difluorophenyl)(thiazol-2-yl)methanone

HRID 741806ノート

反応式

HRID 741806 の反応式
N1C=CC=CC=1.[F:7][C:8]1[CH:9]=[C:10]([CH:15]([C:17]2[S:18][CH:19]=[CH:20][N:21]=2)[OH:16])[CH:11]=[C:12]([F:14])[CH:13]=1>C(Cl)Cl>[F:7][C:8]1[CH:9]=[C:10]([C:15]([C:17]2[S:18][CH:19]=[CH:20][N:21]=2)=[O:16])[CH:11]=[C:12]([F:14])[CH:13]=1

参加物

4

反応物 2

HCID 1049PyridineHCID 194269623,5-Difluoro-alpha-(thiazol-2-yl)benzenemethanol

生成物 1

HCID 19426944(3,5-Difluorophenyl)(thiazol-2-yl)methanone収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of CrO3 (1.1 g, 11 mmol) in CH2Cl2 at r.t. was added pyridine (1.8 mL, 22 mmol) and the resulting mixture was stirred for 20 min.. The alcohol from Step 1 in CH2Cl2 was added and the resulting mixture was stirred for 16 h. Then ET2O was added and the resulting mixture was filtered through silica gel and washed with Et2O. After evaporation the residue was chromatographed on silica gel eluting with 7:3 mixture of hexane:EtOAc to give 1.66 g (90%) of the title compound.

後処理

  1. stirringthe resulting mixture was stirred for 16 h
  2. additionThen ET2O was added
  3. filtrationthe resulting mixture was filtered through silica gel
  4. washwashed with Et2O
  5. customAfter evaporation the residue
  6. customwas chromatographed on silica gel eluting with 7:3 mixture of hexane

出典と根拠

ORDレコード
ord-768d9f1bfd10421f92c5fd709e071b5b
出典データセット
uspto-grants-1996_09
特許番号
US05552437

反応ノート

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