HRID914292

反应详情

EQUATION

反应方程式

HRID 914292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-{[4-(2-Hydroxyethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid tert-butyl ester (451 mg) synthesized in Example 4 and 4′-fluorobiphenyl-4-ol (280 mg) were dissolved in tetrahydrofuran (10 mL), triphenylphosphine (430 mg) and diisopropyl azodicarboxylate (40% toluene solution, 0.88 ml) were added under ice-cooling, and the mixture was stirred at room temperature for 17 hr. The reaction mixture was concentrated under reduced pressure, and hexane (about 10 mL) was added. The precipitated crystals were removed by filtration, and the solvent of the filtrate was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=4:1) to give the title compound (390 mg) as a colorless oil.

WORKUP

后处理

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and hexane (about 10 mL)
  3. additionwas added
  4. customThe precipitated crystals were removed by filtration
  5. customthe solvent of the filtrate was evaporated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=4:1)