HRID30608

反应详情

EQUATION

反应方程式

HRID 30608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of formaldehyde (37% w/w, 8.2 mL) was added to a solution of 4′-Hydroxy acetophenone (100 mmol), and N-methylpiperazine (110 mmol) in EtOH. Heated at reflux overnight. The solvent was evaporated on celite and the residue was purified by flash chromatography and crystallized from heptane to give the title product as white needles in 55% yield. 1H-NMR (DMSO-d6) δ 7.76 (dd, 1H), 7.74 (s, 1H), 6.81 (d, 1H), 3.69 (s, 2H), 2.47 (br, 4H), 2.46 (s, 3H), 2.35 (br, 4H), 2.17 (s, 3H).

WORKUP

后处理

  1. temperatureHeated
  2. temperatureat reflux overnight
  3. customThe solvent was evaporated on celite
  4. customthe residue was purified by flash chromatography
  5. customcrystallized from heptane