HRID16179

反应详情

EQUATION

反应方程式

HRID 16179 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 trans-2,2,2-trifluoro-N-[2,3,4,14b-tetrahydro-7-[(phenylmethyl)amino]-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl]acetamide (944 mg, 2.0 mmol) in ethanol (16 mL) were added Pd/C 10% (111 mg) and a solution of 4M HCl in dioxane (778 μl, 3.11 mmol). The resulting reaction mixture was hydrogenated at 3 bar for 6 h. The reaction mixture was quenched with sat. NaHCO3 (aq) and diluted with ethanol. After filtration through dicalite and thorough washing with ethyl acetate, the volatiles were removed in vacuo. A part of the crude product was purified with HPLC to afford the title compound (29 mg, 53%). Data (m/z)=378 (M+H)+.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. customThe reaction mixture was quenched with sat. NaHCO3 (aq)
  3. additiondiluted with ethanol
  4. filtrationAfter filtration through dicalite
  5. washthorough washing with ethyl acetate
  6. customthe volatiles were removed in vacuo
  7. customA part of the crude product was purified with HPLC