反应详情

温度

0 °C

4.9 g of 2-(3-oxetan-3-yl-phenyl)-ethanol were dissolved in 30 ml of DCM and 9.5 ml of pyridine were added at room temperature. The mixture was cooled to 0° C. and 6.3 g of p-toluenesulfonyl chloride were added at 0° C. Stirring was continued for 6 h at room temperature. Then the volatiles were evaporated, the residue was dissolved in 100 ml of EA and washed with 100 ml of a saturated aqueous solution of sodium hydrogencarbonate. The aqueous layer was extracted two times with 100 ml each of EA. The combined organic layers were dried with magnesium sulfate and evaporated. Silica gel chromatography (EA/HEP 1:1) of the residue yielded 2.0 g of the title compound.

1. customThen the volatiles were evaporated
2. dissolutionthe residue was dissolved in 100 ml of EA
3. washwashed with 100 ml of a saturated aqueous solution of sodium hydrogencarbonate
4. extractionThe aqueous layer was extracted two times with 100 ml each of EA
5. dry with materialThe combined organic layers were dried with magnesium sulfate
6. customevaporated