HRID660684

反应详情

EQUATION

反应方程式

HRID 660684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture is concentrated
  2. custompartitioned between EtOAc and 1N HCl
  3. washThe combined organic layers are washed with saturated sodium bicarbonate and brine
  4. customdried
  5. customevaporated
  6. customto afford a crude orange oil which
  7. customis purified by flash chromatography