HRID1859634

反应详情

EQUATION

反应方程式

HRID 1859634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 25 mL ovendried flask 2-iodophenol (1.03 g, 4.7 mmol) and potassium carbonate (0.71 g, 5.2 mmol) were dissolved in dry acetone (10 mL). The mixture was stirred for 15 min followed by addition of benzylbromide (0.61 mL, 5.2 mmol) and left over-night at rt. Addition of H2O (50 mL) followed by extraction with ethyl acetate (3×50 mL) and the combined organic phases were dried (MgSO4) and evaporated to dryness, to produce 1.7 g of crude 25. The crude product was subjected to CC [eluent: Heptane:EtOAc (9:1)] to give pure 25 (1.2 g, 81%). LC-MS [M+H]+ 310 (cald. 310.0).

WORKUP

后处理

  1. waitleft over-night at rt
  2. extractionfollowed by extraction with ethyl acetate (3×50 mL)
  3. dry with materialthe combined organic phases were dried (MgSO4)
  4. customevaporated to dryness
  5. customto produce 1.7 g of crude 25