HRID1200007

反应详情

EQUATION

反应方程式

HRID 1200007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4.54 g (20 mmol) of 3-hydroxy-2-phenyl-7-azabenzo[b]thiophene and 2.75 g (22 mmol) of potassium t-butoxide in 50 mL of tetrahydrofuran was stirred until the solid dissolved. Then 2.0 g (25 mmol) of chloromethyl methyl ether was added and the solution was stirred at room temperature for 2 hours. The solution was partitioned between ether and water and the aqueous layer was washed with two portions of ether. The ether extracts were washed with brine, dried over MgSO4, and concentrated to 4.33 g (80%) of an oil that crystallized upon standing, m.p. 54° C.

WORKUP

后处理

  1. dissolutiondissolved
  2. stirringthe solution was stirred at room temperature for 2 hours
  3. customThe solution was partitioned between ether and water
  4. washthe aqueous layer was washed with two portions of ether
  5. washThe ether extracts were washed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated to 4.33 g (80%) of an oil that
  8. customcrystallized