HRID1944639

反应详情

EQUATION

反应方程式

HRID 1944639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

41 (220 mg, 0.55 mmol) was dissolved in 15 mL of anhydrous dichloromethane under nitrogen at room temperature. Aluminium chloride (147 mg, 1.1 mmol) was added and the reaction mixture was stirred for 10 minutes. 10 mL of water was added and the product was extracted in dichloromethane (2×20 mL) and the combined organic phases were dried over anhydrous sodium sulfate, evaporated under reduced pressure purified by column chromatography. The product 3, 81 mg (41% yield) was obtained in 10% ethylacetate in hexanes. Rf: 0.54 (60:40 Hex:EA).

WORKUP

后处理

  1. extractionthe product was extracted in dichloromethane (2×20 mL)
  2. dry with materialthe combined organic phases were dried over anhydrous sodium sulfate
  3. customevaporated under reduced pressure
  4. custompurified by column chromatography