HRID1293449

反应详情

EQUATION

反应方程式

HRID 1293449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of Dibenzo[b,d]furan-4-ol (1 g, 5.43 mmol) in DMF (5 ml) was added to a stirred and cooled (0° C.) suspension of 60% sodium hydride (326 mg, 8.12 mmol) in DMF (20 ml). The mixture was stirred at 0° C. for 5 min and cyclopropylmethyl bromide (1.31 g, 10.85 mmol) in DMF (5 ml) was added dropwise over a period of 10 min. The cooling bath was removed and the mixture was stirred for 1 h at room temperature. The reaction mixture was diluted with ice-cold water (100 ml) and extracted with EtOAc (3×50 ml). The combined organic extracts were washed with water (2×100 ml), brine (100 ml) and dried (Na2SO4), to give 1.16 g (90%) of the product as viscous liquid

WORKUP

后处理

  1. temperaturecooled
  2. stirringThe mixture was stirred at 0° C. for 5 min
  3. customThe cooling bath was removed
  4. stirringthe mixture was stirred for 1 h at room temperature
  5. additionThe reaction mixture was diluted with ice-cold water (100 ml)
  6. extractionextracted with EtOAc (3×50 ml)
  7. washThe combined organic extracts were washed with water (2×100 ml), brine (100 ml)
  8. dry with materialdried (Na2SO4)