반응 #159582

반응 방정식

4-fluorophenol

acetonitrile

1-benzhydrylazetidin-3-yl methanesulfonate

→

1-benzhydryl-3-(4-fluorophenoxy)azetidine

반응 조건

후처리

1. 1
   기타The reaction mixture was evaporated in vacuo
2. 2
   추출The aqueous layer was extracted with diethylether (2×10 ml)
3. 3
   기타The organics after solvent evaporation
4. 4
   세척eluting with a mixture cyclohexane/ethylacetate (from 100/0 to 85/15
5. 5
   기타Collected fractions gave
6. 6
   기타after evaporation

실험 절차

To a stirred solution of 4-fluorophenol (0.80 g, 7.16 mmol) in acetonitrile (15 ml) potassium carbonate (1.3 g, 9.30 mmol) was added followed by the addition of 1-benzhydrylazetidin-3-yl methanesulfonate (D19) (2.5 g, 7.87 mmol) and the mixture was stirred under microwave irradiation at 100° C. for 5 mins. The reaction mixture was evaporated in vacuo and the residue was taken up in a mixture diethylether/water (10 ml/10 ml). The aqueous layer was extracted with diethylether (2×10 ml). The organics after solvent evaporation were loaded on SPE-Si (25 g) cartridge eluting with a mixture cyclohexane/ethylacetate (from 100/0 to 85/15. Collected fractions gave, after evaporation, the title compound (D21) (1.8 g).

출처