反应 #1851983

ord-58be4f3deb1344229084f288ffb32d2e

反应条件

温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was cooled
  2. 2
    workup.STIRRINGAfter stirring for 10 minutes
  3. 3
    萃取the water mixture was extracted with ether (3×100 mL)
  4. 4
    洗涤The ether layer was washed with brine (100 mL)
  5. 5
    干燥dried over MgSO4
  6. 6
    过滤filtered
  7. 7
    浓缩concentrated to a residue

实验过程

To a cold boron trifluoride etherate (280 mmol) solution was added 3-fluorophenol or phenol (89 mmol) and 4-chlorobutyryl chloride (178 mmol). The resulting solution was stirred at 130° C. for 18 hours. The reaction mixture was cooled and poured into ice water (100 mL). After stirring for 10 minutes, the water mixture was extracted with ether (3×100 mL). The ether layer was washed with brine (100 mL), dried over MgSO4, filtered and concentrated to a residue to afford 4-chloro-1-(4-fluoro-2-hydroxyphenyl)butan-1-one and 4-chloro-1-(2-hydroxyphenyl)butan-1-one in 52%-67% yield, which was used in the following step without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE039680E1uspto-grants-2007_06