HRID898133

反应详情

EQUATION

反应方程式

HRID 898133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Hydroxy-hex-3-yn-2-one (2 g, 18 mmol) and 2-hexyl-isothiourea hydrobromide (5.2 g, 21 mmol) were dissolved in THF (10 mL). Then the triethylamine (5.5 mL, 40 mmol) was added and stirring continued for 3 h. The reaction was slightly exothermic. The mixture was extracted with AcOEt and sat. NH4Cl solution. The crude product was purified by chromatography on silica gel with a heptane/AcOEt gradient. One obtained 2.8 g (61%) of a light yellow oil. MS: m/z=254 (M)

WORKUP

后处理

  1. extractionThe mixture was extracted with AcOEt and sat. NH4Cl solution
  2. customThe crude product was purified by chromatography on silica gel with a heptane/AcOEt gradient