HRID660684
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
To 5-[4-(2-aminoethyl)-2-benzyloxyphenyl]-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one (0.25 g, 0.434 mmol) (Example 67, step A) in 5 mL dioxane is added triethylamine (0.12 mL, 0.87 mmol), followed by cyclohexyl isocyanate (0.11 mL, 0.87 mmol) and the mixture heated to 85° C. for 1 h. The reaction mixture is concentrated and then partitioned between EtOAc and 1N HCl. The combined organic layers are washed with saturated sodium bicarbonate and brine, dried, and evaporated to afford a crude orange oil which is purified by flash chromatography to afford the title compound as a foam.
WORKUP
后处理
- concentrationThe reaction mixture is concentrated
- custompartitioned between EtOAc and 1N HCl
- washThe combined organic layers are washed with saturated sodium bicarbonate and brine
- customdried
- customevaporated
- customto afford a crude orange oil which
- customis purified by flash chromatography