反应 #49751

ord-9d0abb7cc6254bdbb0310c2c9d07c792

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while refluxing
  2. 2
    其他After completion of the reaction
  3. 3
    萃取extracted with ethyl acetate (50 ml×3 times)
  4. 4
    其他The organic layer was dried
  5. 5
    浓缩concentrated under reduced pressure

实验过程

Ethyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate (1.45 g, 4.97 mmol) prepared by the process described in Reference Example 1 and a solution of potassium carbonate (1.03 g, 7.46 mmol) in ethanol (5.0 ml) were stirred for 1 hour while refluxing, and then cyclopentyl bromide (1.11 g, 7.46 mmol) was added thereto, followed by further stirring for 2 hours. After completion of the reaction, the mixture was poured into 1N hydrochloric acid (50 ml), and extracted with ethyl acetate (50 ml×3 times). The organic layer was dried, and concentrated under reduced pressure to obtain ethyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate as grey white crystals (1.41 g, 4 69 mmol 94.4% yield) The spectral data and the like are as shown in Reference Example 1.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05424277uspto-grants-1995_06