HRID1159792

反应详情

EQUATION

反应方程式

HRID 1159792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Bromo-7-methoxy indole (2 g, 8.8 mmol) was dissolved in CH2Cl2 (300 mL). PhSO2Cl (2.4 g, 9.4 mmol was added, followed by tetrabutylammonium hydrogen sulfate (0.34 g, 0.88 mmol) and 4M aqueous NaOH (17 mL), in that order. The reaction mixture was stirred at ambient temperature for 3 hrs. The layers were separated and the aqueous layer was extracted with CH2Cl2, washed with H2O, dried over Na2SO4, filtered and concentrated. The crude material was recrystallised from ethanol to give 4-bromo-7-methoxy-1-(phenylsulfonyl)-1H-indole, 0.9 g.

WORKUP

后处理

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with CH2Cl2
  3. washwashed with H2O
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude material was recrystallised from ethanol