HRID2203346

反应详情

EQUATION

反应方程式

HRID 2203346 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the intermediate from Step B (5.96 g, 56.7 mmol) in MeOH (35 mL) was added 6N HCl (20.89 mL, 125 mmol) followed by Pd/C (0.905 g, 8.51 mmol). The reaction mixture was kept on Parr shaker for 2 hours at 40 psig hydrogen. The reaction mixture was filtered through Celite™ (diatomaceous earth) and washed with 600 mL of MeOH and the filtrate concentrated. The residue was azeotroped several times with toluene. A dark brown solid was obtained. m/z=110 (M+H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Celite™ (diatomaceous earth)
  2. washwashed with 600 mL of MeOH
  3. concentrationthe filtrate concentrated
  4. customThe residue was azeotroped several times with toluene
  5. customA dark brown solid was obtained