HRID2358115

反应详情

EQUATION

反应方程式

HRID 2358115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 4-[2-fluoro-3-(methylsulfonyl)-phenyl]piperidine-1-carboxylate (0.7 g, 2.2 mmol) in ethanol (4 ml), hydrochloric acid (3 M, 10 ml) was added and the mixture was heated at reflux for 24 h. The ethanol was evaporated and the aqueous residue was basified with sodium hydroxide (5 M) and extracted with ethylacetate (3×50 ml). The combined organic phases was washed with brine (50 ml), dried (MgSO4) and evaporated to dryness to give the title compound (0.5 g, 91%). MS m/z (relative intensity, 70 eV) 257 (M+, 6), 237 (95), 208 (83), 173 (bp) 130 (69).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 24 h
  3. customThe ethanol was evaporated
  4. extractionextracted with ethylacetate (3×50 ml)
  5. washThe combined organic phases was washed with brine (50 ml)
  6. dry with materialdried (MgSO4)
  7. customevaporated to dryness