反应 #58666

ord-b35b30713ad8435ca0fdaf1c324a6c9c

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was cooled
  2. 2
    过滤filtered
  3. 3
    其他The filtrate was partitioned between water and EtOAc
  4. 4
    萃取the aqueous layer was extracted with EtOAc
  5. 5
    洗涤The combined organic layer was washed with brine
  6. 6
    其他dried
  7. 7
    浓缩concentrated
  8. 8
    其他The residue was purified on a flash column

实验过程

To a solution of 1.45 g (9.07 mmol) of 1-(3-cyanophenyl)acetone in 18 mL acetonitrile, 1.1 mL (9.5 mmol) cyclobutyl bromide and 5.91 g (18.1 mmol) cesium carbonate were added. After heating the solution in a 60° C. bath overnight, it was cooled and filtered. The filtrate was partitioned between water and EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layer was washed with brine, dried and concentrated. The residue was purified on a flash column using a gradient of 5-10% EtOAc/hexane to isolate the title compound. 1H NMR: (500 MHz, CDCl3): δ 1.5-2.2 (m, 9H), 2.13 (s, 3H), 3.64 (m, 1H), 7.4-7.7 (m, 4H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07423067B2uspto-grants-2008_09