HRID263218

反应详情

EQUATION

反应方程式

HRID 263218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of phenol (18.8 g) and sodium hydroxide (8 g) was stirred at 60°-70° in dimethylformamide (162 ml) and water (18 ml) while 1-bromo-3-methylbut-2-ene (VII, R1 =R2 =CH3, Hal=Br) (29.8 g) was added dropwise over 11/2 h. The mixture was stirred at 60° for 4 h after the addition was complete. It was then poured into water (800 ml) and extracted with ether (3×300 ml). The ether extract was washed with 10% sodium hydroxide (200 ml) and then with water (3×200 ml) before drying over anhydrous sodium sulphate. The solvent was removed in vacuo, and the residue distilled to give 1-phenoxy-3-methylbut-2-ene (2.4 g, yield 75%) as a clear liquid b.p. 116°-118°/18 mm. Hg.

WORKUP

后处理

  1. additionafter the addition
  2. extractionextracted with ether (3×300 ml)
  3. extractionThe ether extract
  4. washwas washed with 10% sodium hydroxide (200 ml)
  5. dry with materialwith water (3×200 ml) before drying over anhydrous sodium sulphate
  6. customThe solvent was removed in vacuo
  7. distillationthe residue distilled