HRID131626

反应详情

EQUATION

反应方程式

HRID 131626 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 ethyl 3-methyl-1-(2-methylpropyl)-2,4-dioxo-1,2,3,4-tetrahydro-thieno[2,3-d]pyrimidine-5-carboxylate (1.5 g), 2,4-dichlorothiazole-5-carboxaldehyde (1.75 g) and DMPU (1.2 ml) in THF (25 ml) at −78° C., was added LDA (10 mmol). Acetic acid (3 ml) was added and the mixture allowed to warm to ambient temperature. The mixture was then partitioned between ethyl acetate and water, the organics were collected, dried over magnesium sulphate and concentrated to dryness. The residue was purified by normal phase chromatography (3:1 i-hexane:ethyl acetate) to give the sub-title compound as a yellow foam (0.45 g).

WORKUP

后处理

  1. customThe mixture was then partitioned between ethyl acetate and water
  2. customthe organics were collected
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated to dryness
  5. customThe residue was purified by normal phase chromatography (3:1 i-hexane:ethyl acetate)