反应 #1869212

ord-ef69b6f7495e473da852aa96bc95b40c

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe reaction mixture was stirred at room temperature over the week-end
  2. 2
    干燥The organic layer was dried over Na2SO4
  3. 3
    过滤filtered
  4. 4
    浓缩concentrated
  5. 5
    其他The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit)

实验过程

A mixture of (2,4-dimethoxyphenyl)acetic acid (577 mg, 3.0 mmol) and N,N-carbonyldiimidazole (608 mg, 3.75 mmol) in DMF (10 mL) was stirred at room temperature for 45 min, aqueous 40% methyl amine (4.5 mL) was added and the reaction mixture was stirred at room temperature over the week-end. The reaction mixture was is partitoned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit) to give the subtitled compound (460 mg).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07498338B2uspto-grants-2009_03