HRID1084967
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter 1 h the solvent was evaporated
- customthe residue was partitioned between 8% sodium bicarbonate (20 ml) and ethyl acetate (20 ml)
- washThe organic layer was washed with water and brine
- customdried
- concentrationconcentrated in vacuo
- customto give a yellow solid which
- customwas triturated with ether