HRID1111938

反应详情

EQUATION

反应方程式

HRID 1111938 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 gm of 1-(4'-amino-3'-bromo-5'-trifluoromethyl-phenyl)-2-tert.pentylamino-ethanol hydrochloride were distributed between ethyl acetate and 2N ammonia. The organic layer was dried and evaporated in vacuo, the residual base was dissolved in 100 ml of methanol in a hydrogenation vessel. 2.5 gm of palladium oxide/barium sulfate catalyst (5%) were added, and the mixture was hydrogenated until 1 mol of hydrogen had been absorbed. After the catalyst had been removed by filtration, the filtrate was evaporated in vacuo, and the solid residue was recrystallized from isopropanol. The obtained hydrobromide melted at 174°-175° C. (decomp.).

WORKUP

后处理

  1. customThe organic layer was dried
  2. customevaporated in vacuo
  3. dissolutionthe residual base was dissolved in 100 ml of methanol in a hydrogenation vessel
  4. addition2.5 gm of palladium oxide/barium sulfate catalyst (5%) were added
  5. customhad been absorbed
  6. customAfter the catalyst had been removed by filtration
  7. customthe filtrate was evaporated in vacuo
  8. customthe solid residue was recrystallized from isopropanol