HRID33223

反应详情

EQUATION

反应方程式

HRID 33223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-[1,3]Dioxan-2-yl-butyric acid methyl ester (6.8 g, 0.036 mol) was added to a stirred solution of sodium hydroxide (1.87 g, 0.047 mol) in water (30 ml) and methanol (30 ml). The mixture was stirred for 18 h at room temperature and then the solvent evaporated. The residue was partitioned between ethyl acetate (100 ml) and water (100 ml) and cooled to 0° C. The mixture was acidified with hydrochloric acid (1M) to pH 2 and the layers separated. The aqueous layer was further extracted with cold ethyl acetate (100 ml) and the combined organic layers washed with brine (100 ml) and then dried (Na2SO4). The solvents were evaporated and the crude solid (5.56 g) was used in the next step.

WORKUP

后处理

  1. customthe solvent evaporated
  2. customThe residue was partitioned between ethyl acetate (100 ml) and water (100 ml)
  3. temperaturecooled to 0° C
  4. customthe layers separated
  5. extractionThe aqueous layer was further extracted with cold ethyl acetate (100 ml)
  6. washthe combined organic layers washed with brine (100 ml)
  7. dry with materialdried (Na2SO4)
  8. customThe solvents were evaporated