HRID514795

反应详情

EQUATION

反应方程式

HRID 514795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-Methoxy-1,2-dihydro-6H-cyclopenta[c]carbazole-3-one (82) (27.8 g, 110.8 mmol, 1 eq) was dissolved in dry dichloromethane (300 mL). Anhydrous AlCl3 (29.5 g, 221.5 mmol, 2 eq) was added in portions with stirring and cooling, followed by the dropwise addition of AcCl (24 mL, 332.4 mmol, 3 eq). The reaction mixture was stirred at about 5° C. for 24 h and poured into ice water (violent foaming should be avoided). The precipitated orange solid was filtered off, washed with water (10×100 mL), CH2Cl2 (3×50 mL), acetone (3×50 mL) to give 26 g (80%) of 9-acetyl-8-methoxy-1,2-dihydro-6H-cyclopenta[c]carbazole-3-one (83).

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe reaction mixture was stirred at about 5° C. for 24 h
  3. filtrationThe precipitated orange solid was filtered off
  4. washwashed with water (10×100 mL), CH2Cl2 (3×50 mL), acetone (3×50 mL)