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0 °C

A concentrated solution of the amine 18 (0.17 g, 0.17 mmol) in ethyl acetate was added cooled to 0° C. A total of 4 mL of a freshly prepared saturated solution of HCl in ethyl acetate was added dropwise and the solution stirred for 1 h at room temperature during which time a white precipitate formed. The ethyl acetate was removed in vacuo and the residue co-evaporated with ethyl acetate and chloroform to give the product 25 as a white powder (0.151 g, 98%); 1H NMR (CDCl3/CH3OD 9:1) d 7.13 (s, 1H, aryl), 7.02 (d, 1H, aryl), 6.85 (d, 1H, aryl), 5.33 (m, 4H, olefinic), 4.05 (m, 2H, benzylic), 3.97 (t, 2H, OCH2), 3.04 (m, 6H, 3×CH2) 2.93 (m, 2H, CH2), 2.02 (m, 8H, CH2C═C), 1.90 (m, 8H, 4×CH2), 1.81 (m, 4H, CH2CH2O), 1.47 (m, 4H, 2×CH2), 1.40-1.17 (m, 40H, 20×CH2), 0.89 (t, 6H, CH3); 13C NMR (300 MHz, D2O) δ 148.94, 148.33, 129.26, 129.19, 123.64, 122.52, 113.10, 68.50, 68.39, 49.96, 45.98, 45.43, 39.86, 31.28, 29.18, 29.11, 28.93, 28.86, 28.70, 28.62, 26.64, 26.59, 25.68, 25.62, 24.00, 22.54, 22.46, 22.11, 13.89; HRMS (FAB): theory for C51H96N3O2 (M+1), 782.7497; found (M+1), 782.7495; Anal. (C51H95Cl3N3O2.0.6H2O): C, H, N.

1. customformed
2. customThe ethyl acetate was removed in vacuo