HRID21473

反应详情

EQUATION

反应方程式

HRID 21473 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.

WORKUP

后处理

  1. temperaturewhile refluxing
  2. customAfter completion of the reaction
  3. extractionextracted with ethyl acetate (50 ml×3 times)
  4. customThe organic layer was dried
  5. concentrationconcentrated under reduced pressure