HRID1084967

反应详情

EQUATION

反应方程式

HRID 1084967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[3-[(6-Bromohexyl)oxy]propyl]benzeneacetamide (950 mg) was added to a stirred solution of 4-amino-α-(aminomethyl)-3,5-dichloro-benzenemethanol (900 mg) and DEA (650 mg) in DMF (10 ml) at 100° under nitrogen. After 1 h the solvent was evaporated and the residue was partitioned between 8% sodium bicarbonate (20 ml) and ethyl acetate (20 ml). The organic layer was washed with water and brine, dried and concentrated in vacuo to give a yellow solid which was triturated with ether to give the title compound as an off-white powder (510 mg) m.p. 104°-106°.

WORKUP

后处理

  1. customAfter 1 h the solvent was evaporated
  2. customthe residue was partitioned between 8% sodium bicarbonate (20 ml) and ethyl acetate (20 ml)
  3. washThe organic layer was washed with water and brine
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customto give a yellow solid which
  7. customwas triturated with ether