1. The layers were quickly separated and the aqueous layer was washed with additional benzene (2 x 7 mL). The combined organics were dried over anhydrous Na2SO4, filtered, and concentrated to dryness in vacuo. The residue was recrystallized from CH2Cl2/Et2O to obtain 22;Benzene Nh4cl;mL) was added
2. 1.11 (d, J = 5.0 Hz, 6H). 19 F NMR (471 MHz, CD2Cl2) ? -118.04. 31 P NMR (202 MHz, CD2Cl2) ? 94;Hz, 4H), 7.58 (t, J = 10.0 Hz, 8H), 7.19 -7.08 (m, 4H), 6.82 (t, J = 10.0 Hz, 4H), 4.06 -3.96 (m, 1H),1018
3. The reaction mixture was stirred at room temperature overnight. Saturated NaHCO3 (15 mL) was added. The aqueous phase was separated and extracted with EtOAc (2 � 10 mL), dried (Na2SO4), filtered and concentrated in vacuo. Purification by column chromatography (petroleum ether/ethyl acetate = 7:1) to afford the title compound S6 (0.93 g, 76 %) as a colorless solid;g, 5 mmol) and Et3N (1.4 mL, 10 mmol) in CH2Cl2 (20 mL) was added Methanesulfonyl chloride (0.78 mL, 10 mmol)
4. IR (ATR): ? = 2999;): 244.1 (M + ),1196