반응 #49751
ord-9d0abb7cc6254bdbb0310c2c9d07c792
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후처리
- 1온도while refluxing
- 2기타After completion of the reaction
- 3추출extracted with ethyl acetate (50 ml×3 times)
- 4기타The organic layer was dried
- 5농축concentrated under reduced pressure
실험 절차
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.