HRID2254117

反应详情

EQUATION

反应方程式

HRID 2254117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 10 mL of absolute ethanol under a nitrogen atmosphere was added 0.15 g of sodium metal. After all the sodium had reacted, 1.00 g of 2-carboethoxycyclohexanone was added followed by 0.78 g of 85% trifluoroacetamidine. The reaction was refluxed gently overnight. The reaction was cooled to room temperature and all solvents were removed by evaporation. The pH of the residue was adjusted to 6 with dilute hydrochloric acid and refluxed briefly and allowed to cool. The resulting solid was collected. (0.73 g, 57%): 1H NMR (DMSO-d6, 300 MHz) δ 13.0 (s, 1H), 2.78 (m, 2H), 2.45 (m, 2H), 1.78 (m, 4H).

WORKUP

后处理

  1. temperatureThe reaction was refluxed gently overnight
  2. customall solvents were removed by evaporation
  3. temperaturerefluxed briefly
  4. temperatureto cool
  5. customThe resulting solid was collected