HEPTAETHYLENE GLYCOL MONOMETHYL ETHER

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared from heptaethylene glycol monomethyl ether (Heimann, U.; Voegtle, F. Liebigs Ann. Chem. 1980, 6, 858-862), methanesulfonyl chloride and ammonium hydroxide using methods similar to those described in Example 101a. The crude product was obtained as a white solid and was used without further purification (2.1 g, 96% yield). 1H-NMR (400 MHz, DMSO-d6) δ:7.3 (br s, 3H), 3.60-3.35 (m, 28H), 3.21 (s, 3H), 2.31 (s, 3H).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared from heptaethylene glycol monomethyl ether (Heimann, U.; Voegtle, F. Liebigs Ann. Chem. 1980, 6, 858-862), methanesulfonyl chloride and ammonium hydroxide using methods similar to those described in Example 101a. The crude product was obtained as a white solid and was used without further purification (2.1 g, 96% yield). 1H-NMR (400 MHz, DMSO-d6) δ:7.3 (br s, 3H), 3.60-3.35 (m, 28H), 3.21 (s, 3H), 2.31 (s, 3H).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared from heptaethylene glycol monomethyl ether (Heimann, U.; Voegtle, F. Liebigs Ann. Chem. 1980, 6, 858-862), methanesulfonyl chloride and ammonium hydroxide using methods similar to those described in Example 101a. The crude product was obtained as a white solid and was used without further purification (2.1 g, 96% yield). 1H-NMR (400 MHz, DMSO-d6) δ:7.3 (br s, 3H), 3.60-3.35 (m, 28H), 3.21 (s, 3H), 2.31 (s, 3H).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 6.7 g (60 mmol) of TEA are dropwise added, in 10 min, to a solution of 13.3 g (60 mmol) of 4-nitrobenzenesulfonyl chloride (marketed product) and of 20.4 g (60 mmol) of 3,6,9,12,15,18,21-heptaoxadocosan-1-ol (according to Liebigs Ann. Chem. 1980, 858-862) in 60 mL of AcOEt. After 2 h at the temperature of 20° C., the precipitated TEA hydrochloride is filtered off, washing with 10 mL of AcOEt for three times. The filtrates are collected, washed with 30 mL of H2O, 20 mL of 2N HCl and then with H2O to reach a neutral pH. The organic phase is evaporated to dryness, to give a thick oil which is directly used in the successive step without a further purification. 25 g (47 mmol) of the desired product are obtained. the precipitated TEA hydrochloride is filtered off washing with 10 mL of AcOEt for three times The filtrates are collected washed with 30 mL of H2O, 20 mL of 2N HCl The organic phase is evaporated to dryness to give a thick oil which is directly used in the successive step without a further purification

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This compound was prepared from heptaethylene glycol monomethyl ether (Heimann, U.; Voegtle, F. Liebigs Ann. Chem. 1980, 6, 858-862), methanesulfonyl chloride and ammonium hydroxide using methods similar to those described in Example 101a. The crude product was obtained as a white solid and was used without further purification (2.1 g, 96% yield). 1H-NMR (400 MHz, DMSO-d6) δ:7.3 (br s, 3H), 3.60-3.35 (m, 28H), 3.21 (s, 3H), 2.31 (s, 3H).