HRID1159824

反应详情

EQUATION

反应方程式

HRID 1159824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-[-2-(3-Benzyloxy-6-bromo-2-nitro-phenyl)-vinyl]-pyrrolidine (10 g, 24.8 mmol; Intermediate 82) suspended in HOAc (25 mL) was added to a boiling mixture of iron (4.15 g, 74.4 mmol) in HOAc. After 2 h boiling TLC indicated that no starting material is left. The reaction mixture was filtered while still warm. The residue was evaporated and dissolved in toluene. The toluene slurry was applied to a silica column and eluted with toluene/hexane 1/1. Obtained 3.1 g. MS (ESI+) for C15H12BrNO m/z 302, 304 (M+H)+.

WORKUP

后处理

  1. waitis left
  2. filtrationThe reaction mixture was filtered
  3. temperaturewhile still warm
  4. customThe residue was evaporated
  5. dissolutiondissolved in toluene
  6. washeluted with toluene/hexane 1/1
  7. customObtained 3.1 g