HRID536468

反应详情

EQUATION

反应方程式

HRID 536468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of Example 28A (780 mg, 4.45 mmol) in 7M NH3 in MeOH (5.00 mL) was added to Ra—Ni 2800 water slurry (1.56 g, 26.6 mmol) in a 50 mL pressure bottle. The reaction mixture was and stirred for 10 hours at 30 psi at ambient temperature. After 3 hours, the solution was filtered and concentrated. The resulting residue was purified by silica gel chromatography (gradient elution: 1-15% MeOH/CH2Cl2 with 1% NH4OH) to provide the title compound. MS (DCI+) m/z 182 (M+H)+.

WORKUP

后处理

  1. waitAfter 3 hours
  2. filtrationthe solution was filtered
  3. concentrationconcentrated
  4. customThe resulting residue was purified by silica gel chromatography (gradient elution: 1-15% MeOH/CH2Cl2 with 1% NH4OH)