HRID1830162

反应详情

EQUATION

反应方程式

HRID 1830162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Compound 3 (9.0 g, 39 mmol) was dissolved in ethanol (100 ml) and water (20 ml) followed by the addition of 9 grams of Pd(OH)2 and TFA (4 ml). The mixture was hydrogenated at 50 psi for 48 hours, then the reaction was filtered through celite which was concentrated to give 9 grams of crude material 4 which was used without further purification. Compound 4 was dissolved in dry methanol (300 ml) and HCl gas was bubbled through for 15 minutes. The reaction was stirred at room temperature for three days and was concentrated. The crude product was purified on silica eluting With 1:1 heptane/ethyl acetate to give 3.9 grains of compound 5.

WORKUP

后处理

  1. filtrationthe reaction was filtered through celite which
  2. concentrationwas concentrated
  3. customto give 9 grams of crude material 4 which
  4. customwas used without further purification
  5. dissolutionCompound 4 was dissolved in dry methanol (300 ml)
  6. customHCl gas was bubbled through for 15 minutes
  7. concentrationwas concentrated
  8. customThe crude product was purified on silica eluting With 1:1 heptane/ethyl acetate