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

HRID 741806노트

반응식

HRID 741806 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-768d9f1bfd10421f92c5fd709e071b5b
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05552437

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