“…mp 107-111 °C (from methanol); Rf: 0.55 (silica gel TLC, methanol-CH2Cl2 1:5); IR (KBr) νmax 3424 (br), 1604,1590,1580,1510,1478,1441,1340,1276,1143,1096,1072,1034,972,893,756, 565 cm -1 ; 1 H-NMR (300 MHz, CD3OD, 25 °C): δ = 3.50-3.53 (m, 2H, OCH2), 3.65-3.73 (m, 12H, OCH2), 3.76 (s, 3H, complexed MeOH), 3.94-3.97 (m, 2H, OCH2), 6.88 (dd, J = 8.0 Hz, 5.7 Hz, 1H, ArH), 7.03 (dd, J = 9.0 Hz, 5.2 Hz, 2H, ArH), 7.35-7.40 (m, 1H, ArH), 7.93 (ddd, J = 13.5 Hz, 7.5 Hz, 1.5 Hz, 1H, ArH), 8.29 (dd, J = 9.1 Hz, 2.9 Hz, 1H, ArH), 8.88 (dd, J = 13.4 Hz, 2.9 Hz, 1H, ArH) ppm; 13 C-NMR (75 MHz, CD3OD, 25 °C): δ = 56. 5,61.7,68.0,70.6,70.6,70.9,71.2,73.4 (OCH2) 4. 7,9,10,12,13,15,4,7,10,13,16]pentaoxa-λ 5 -phosphacyclooctadecin-22-one (4) Macrocycle 13 (0.20 g, 0.38 mmol), dioxane (15 mL), aqueous HCl (15 mL).…”