HRID1081297

反应详情

EQUATION

反应方程式

HRID 1081297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

72 g of 5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 16a were dissolved in 500 ml of tetrahydrofuran, and hydrogenated using 5 g of palladium on carbon (5%) for 5 hours at room temperature with 15 to 20 bar of hydrogen. The mixture was then filtered and the solvent stripped off in vacuo. The yield was 60 g (93% of theory), the boiling point was 80° to 82° C. at 0.1 mbar. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -66.5 and -79.4 ppm; 1H-NMR: 4.68 ppm.

WORKUP

后处理

  1. customfor 5 hours
  2. customat room temperature
  3. filtrationThe mixture was then filtered