HRID5213

反应详情

EQUATION

反应方程式

HRID 5213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(3-Bromopropyl)benzene (20 g) in THF (75 ml) was added dropwise to magnesium (2.43 g) at a rate to maintain gentle reflux. The mixture was stirred for 2 h at RT and oxetane (10 g) was added dropwise. The resulting suspension was stirred at RT for 2h and at reflux for 16 h and poured into saturated aqueous NH4Cl (100 ml). The mixture was extracted with ER (3×75 ml) and the dried extract was evaporated to leave a yellow oil. Distillation of the oil gave the title compound as a colourless liquid (6.05 g) b.p. 100-105°/0.4 mmHg. T.l.c. [O] 0.3.

WORKUP

后处理

  1. temperatureto maintain gentle reflux
  2. temperatureat reflux for 16 h
  3. extractionThe mixture was extracted with ER (3×75 ml)
  4. extractionthe dried extract
  5. customwas evaporated
  6. customto leave a yellow oil
  7. distillationDistillation of the oil