반응 #488899

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64b

Methyl 4-(2-phenyl-1,3-dithiolan-2-yl)benzoate

Selectfluor

HF-pyridine

→

compound 64c

Methyl 4-(difluoro(phenyl)methyl)benzoate

용매

CH2Cl2

CH2Cl2

polyethylene

반응 조건

후처리

1. 1
   기타the consumption of all 64b
2. 2
   workup.ADDITIONthe reaction was diluted with CH2Cl2
3. 3
   건조The combined organics were dried over anhydrous Na2SO4
4. 4
   농축concentrated
5. 5
   기타The crude product was purified by flash column chromatography (silica gel, 5% EtOAc/hexanes)

실험 절차

Selectfluor (1.07 mmol, 381 mg) and HF-pyridine reagent (1.5 mL, HF: Pyridine=70:30 wt %) were dissolved in CH2Cl2 (4 mL) in a polyethylene bottle and cooled to 0° C. A solution of 64b (0.512 mmol, 162 mg) in CH2Cl2 (2 mL) was slowly added and the mixture was stirred for 45 min at room temperature. When TLC indicated the consumption of all 64b, the reaction was diluted with CH2Cl2. The combined organics were dried over anhydrous Na2SO4 and concentrated. The crude product was purified by flash column chromatography (silica gel, 5% EtOAc/hexanes) to afford compound 64c as a clear oil.

출처