HRID2279946

反应详情

EQUATION

反应方程式

HRID 2279946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 2-[5-(hydroxymethyl)-2-thienyl]acetate in tetrahydrofuran (10 mL) and methanol (10 mL) was added 1 N aqueous solution of lithium hydroxide (11.83 mL) and the resulting solution was stirred at room temperature for 4 h. The reaction mixture was cooled to 0° C. and acidified to pH 1 with 2 N aqueous solution of HCl. The solution was concentrated in vacuo and the residue partitioned between ethyl acetate (30 mL) and water (30 mL). The organic phases were dried over magnesium sulfate, filtered and concentrated in vacuo to give the title compound as an orange solid (1.02 g, quantitative yield) which was used in the next step without further purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. concentrationThe solution was concentrated in vacuo
  3. customthe residue partitioned between ethyl acetate (30 mL) and water (30 mL)
  4. dry with materialThe organic phases were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo