反应 #2460343

ord-46b221d9f10a44a0abcf4ea8d67843c1

反应条件

温度
85°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the suspension was filtered
  2. 2
    洗涤washed thoroughly with ethanol
  3. 3
    浓缩The filtrate was concentrated under reduced pressure
  4. 4
    洗涤the resulting solid was washed with EtOAc
  5. 5
    其他to remove excess 2,4-dichloropyrimidine

实验过程

To a stirred solution of N-(4-aminophenyl)acetamide (5 g, 0.033 mol) and NaHCO3 (5.6 g, 0.067 mol) in THF (20 mL) and ethanol (80 mL) was added 2,4-dichloropyrimidine (5.95 g, 0.04 mol) at room temperature. The reaction was gradually heated to 85° C. After the reaction was stirred for four hours at 85° C. under N2, the suspension was filtered and washed thoroughly with ethanol. The filtrate was concentrated under reduced pressure, and the resulting solid was washed with EtOAc to remove excess 2,4-dichloropyrimidine to yield 8.35 g (95.5% yield) of N-{4-[(2-chloropyrimidin-4-yl)amino]phenyl}acetamide as an off-white solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459455B2uspto-grants-2008_12