HRID1486278

反应详情

EQUATION

反应方程式

HRID 1486278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.00 g (4.00 mmol) of rac-benzyl (2-cyano-4-fluorobutan-2-yl)carbamate from Example 73A were dissolved in 114 ml ethanol/glacial acetic acid (1/1), and 0.85 g of palladium on activated carbon (10%) were added. The reaction mixture was hydrogenated in an autoclave at 30-50 bar for 3 h. The reaction mixture was filtered through a fluted filter, rinsed with ethanol and then filtered once again through a Millipore filter. The filtrate was admixed with 10 ml of hydrogen chloride solution (2 N in diethyl ether) and then concentrated by evaporation. This gave 1.04 g of the target compound which was used in the subsequent stage without further purification.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through
  2. filtrationa fluted filter
  3. washrinsed with ethanol
  4. filtrationfiltered once again through a Millipore
  5. filtrationfilter
  6. concentrationconcentrated by evaporation
  7. customThis gave 1.04 g of the target compound which was used in the subsequent stage without further purification