HRID1375032

反应详情

EQUATION

反应方程式

HRID 1375032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 4,5,6,7-tetrahydrothieno[3,2-c]pyridine (0.86 g), 2-bromoethanol (0.66 g), potassium carbonate (2.58 g) and potassium iodide (3.10 g) in N,N-dimethylformamide (20 ml) was stirred at 70° C. for 2 hours. After cooling, ethyl acetate and water were added thereto. The organic layer was separated, washed with water twice, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using a mixed solvent of methanol and dichloromethane (1:10) as an eluent. The fractions containing the objective compound were collected and evaporated under reduced pressure to give 5-(2-hydroxyethyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine (0.53 g) as an oil.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customThe organic layer was separated
  3. washwashed with water twice
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel using a mixed solvent of methanol and dichloromethane (1:10) as an eluent
  7. additionThe fractions containing the objective compound
  8. customwere collected
  9. customevaporated under reduced pressure