HRID556622

反应详情

EQUATION

反应方程式

HRID 556622 的结构方程式

PROCEDURE

实验过程

The product of Example 48 (300 mg, 0.67 mmol) and trifluoroethylamine (300 mg, 3 mmol) were dissolved in THE (10 ml) and sealed in a vial under Ar. The mixture was heated in an oil bath to 60° for 4 days. The solvents were removed in vacuo, and the residue was flash chromatographed with 60-90% CH2Cl2/hexane. Recrystallization from CH2Cl2/hexane gave the title compound as a white crystalline solid. mp 195-196°, LC MS m/z=465(MH+) Retention time=2.38 min.

WORKUP

后处理

  1. customsealed in a vial under Ar
  2. temperatureThe mixture was heated in an oil bath to 60° for 4 days
  3. customThe solvents were removed in vacuo
  4. customchromatographed with 60-90% CH2Cl2/hexane
  5. customRecrystallization from CH2Cl2/hexane