HRID1055767

反应详情

EQUATION

反应方程式

HRID 1055767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

60 mg (0.195 mmol) of the compound of Example 83A and 60 mg (0.195 mmol) of the compound of Example 19A were dissolved in 2 ml of DMF, and 89 mg (0.234 mmol) of HATU and 41 μl (0.234 mmol) of N,N-diisopropylethylamine were added in succession. After about 16 h of stirring at RT, the reaction mixture was diluted with 1 ml of acetonitrile and separated into its components by preparative HPLC (Method 36). The product fractions were combined and freed from the solvent on a rotary evaporator. The residue was dissolved in a little methanol and the solution was passed through a bicarbonate cartridge (from Polymerlabs, Stratospheres SPE, PL-HCO3 MP SPE, capacity 0.9 mmol) to convert the formate salt obtained after preparative HPLC into the free base. Evaporation and drying under high vacuum gave 42 mg (35% of theory) of the title compound.

WORKUP

后处理

  1. customseparated into its components by preparative HPLC (Method 36)
  2. customfreed from the solvent on a rotary evaporator
  3. dissolutionThe residue was dissolved in a little methanol
  4. customobtained after preparative HPLC into the free base
  5. customEvaporation
  6. customdrying under high vacuum