HRID1251309

反应详情

EQUATION

反应方程式

HRID 1251309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Free base. In a round-bottomed flask equipped with a magnetic stir bar, 6.51 g (12.1 mmol) of N-benzylbis(3-benzenesulfonamidopropyl)amine hydrochloride, 40 mL of CH2Cl2, 15 mL of a solution of 1 N aq. NaOH and 15 mL of saturated aq. NaCl were combined. After stirring vigorously for 30 min, the layers were separated and the organic portion dried (MgSO4). Removal of the drying agent by filtration, concentration of the filtrate by rotary evaporation and further drying under vacuum (0.4 mm, 45° C.) for 24 h afforded 5.96 g (98%) of N-benzylbis (3-benzenesulfonamidopropyl)amine as a thick colorless oil. TLC (silica) : Rf=0.21, 1:1 (v/v) ethyl acetate:hexane. 1H NMR (CDCl3/TMS) δ7.82 (d, 4 H, J=7 Hz,SO2ArH2,6), 7.51 (m, 6 H, SO2ArH3,4,5), 7.22 (m, 3 H, BnArH2,4,6), 7.16 (m, 2 H, BnArH3,5), 5.9 (br, 2 H, SO2NH) 3.40 (s, 2 H, PhCH2N), 2.92 (t, 4 H, SO2NCH2CH2), 2.38 (t, 4 H, BnCH2CH2), 1.62 (quint, 4 H, NCH2CH2CH2N) 13 C NMR (CDCl3) δ139.9, 138.2, 132.4, 129.0, 128.4, 127.2, 126.9, 58.7, 51.8, 42.2, 26.1. IR (NaCl plate, cm−1) 3277 (br), 3061 (w), 1446 (s), 1325 (s), 1160 (s), 1093 (s).

WORKUP

后处理

  1. customIn a round-bottomed flask equipped with a magnetic stir bar
  2. customthe layers were separated
  3. dry with materialthe organic portion dried (MgSO4)
  4. customRemoval of the drying agent
  5. filtrationby filtration, concentration of the filtrate
  6. customby rotary evaporation
  7. customfurther drying under vacuum (0.4 mm, 45° C.) for 24 h