HRID1804631

反应详情

EQUATION

反应方程式

HRID 1804631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2.0 g (12 mmol) of the title compound from Step A in 50 mL of acetone under an atmosphere of nitrogen was added 2.5 g (18 mmol) of potassium carbonate and 2.4 g (14 mmol) of ethyl bromoacetate. The reaction mixture was refluxed overnight. After cooling, the inorganic materials were filtered off and washed with acetone. The filtration was concentrated and purified by MPLC (Biotage Horizone: Flash 65i) eluent: 100% dichloromethane to 12% methanol in dichloromethane to give 2.5 g of the title compound as an oil. LC/MS: (M+1) 240.9

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed overnight
  2. temperatureAfter cooling
  3. filtrationthe inorganic materials were filtered off
  4. washwashed with acetone
  5. filtrationThe filtration
  6. concentrationwas concentrated
  7. custompurified by MPLC (Biotage Horizone: Flash 65i) eluent