HRID46202

反应详情

EQUATION

反应方程式

HRID 46202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 2-(6-(2-chloro-5-((2S,3S,4R,5R,6R)-3,4,5-tris(benzyloxy)-6-(benzyloxymethyl)-tetrahydro-2H-pyran-2-yl)benzyl)pyridazin-3-yl)-5-methyloxazole (1.2 mmol) from Step 2 in acetonitrile (5 mL) was added Iodotrimethylsilane (3 mL). The resulting reaction mixture was heated to 50° C. overnight. After cooling to 0° C., the reaction quenched with methanol and concentrated in vacuo. Purification by reverse phase preparative HPLC (Gilson®, SunFire™ Prep, 5 to 50% acetonitrile in water gradient) provided the title compound (62 mg, 0.14 mmol, 11%) as a yellow solid.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperatureAfter cooling to 0° C.
  3. customthe reaction quenched with methanol
  4. concentrationconcentrated in vacuo
  5. customPurification by reverse phase preparative HPLC (Gilson®, SunFire™ Prep, 5 to 50% acetonitrile in water gradient)