HRID1179515

反应详情

EQUATION

反应方程式

HRID 1179515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4.00 g (20.6 mmol) of 9-aminoacridine 540 in 350 mL of CHCl3 was added 2.9 mL (20.8 mmol) of Et3N and 4.50 g (20.6 mmol) of mesitylenesulfonyl chloride. The reaction mixture was refluxed for 72 hr. Then the reaction mixture was filtered and the solvent was evaporated. The material was purified by column chromatography on silica gel by eluting first with 1% MeOH in CH2Cl2 and then with 5% MeOH in CH2Cl2 to yield 458.4 mg (6%) of sulfonamide 541 as an orange solid: 1H NMR (300 MHz, CDCl3, TMS) δ 9.25 (s, 1H), 8.77 (d, J=8 Hz, 2H), 7.46 (t, J=8 Hz, 2H), 7.21 (d, J=8 Hz, 2H), 7.15 (t, J=8 Hz, 2H), 7.02 (s, 2H), 2.78 (s, 6H), 2.36 (s, 3H).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 72 hr
  2. filtrationThen the reaction mixture was filtered
  3. customthe solvent was evaporated
  4. customThe material was purified by column chromatography on silica gel
  5. washby eluting first with 1% MeOH in CH2Cl2