HRID1274224

反应详情

EQUATION

反应方程式

HRID 1274224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Butyllithium (12.5 ml of 1.6N in hexanes) was added to a stirred solution of thiophene (1.68 g) in dry tetrahydrofuran (80 ml). The mixture was stirred at room temperature for 0.5 h and then a solution of 4-methoxybenzylbromide (2.62 g) in tetrahydrofuran (10 ml) was added dropwise. The mixture was stirred for 1 h and then acetic acid (1.2 ml) was added and the solvent evaporated. The residue was partitioned between ethyl acetate and water, the organic phase was washed with water and brine dried over magnesium sulphate and evaporated. The product was isolated by column chromatography (Kieselgel:hexane). δ(CDCl3) 3.80 (3H, s), 4.10 (2H, s), 6.78-6.94 (4H, m), 7.13-7.20 (3H, m).

WORKUP

后处理

  1. stirringThe mixture was stirred for 1 h
  2. customthe solvent evaporated
  3. customThe residue was partitioned between ethyl acetate and water
  4. washthe organic phase was washed with water and brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe product was isolated by column chromatography (Kieselgel:hexane)