HRID988830

反应详情

EQUATION

反应方程式

HRID 988830 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 2.0 g (5.37 mmol) of the product from Method L and 1.1 grams (13.4 mmol) of piperidine in 10 mL of tert-butanol was heated with stirring at 60° C. for 2 hours. After cooling to room temperature, the reaction mixture was partitioned between dichloromethane (25 mL) and water (25 mL). The dichloromethane layer was dried over sodium sulfate (Na2SO4) and concentrated to dryness in vacuo affording 2.2 grams (97%) of the title compound. 1H NMR (400 MHz) (CDCl3)δ: 1.63-1.72 (m, 6H), 3.54-3.57 (m, 4H), 7.53 (t, 2H, J=2.0 Hz), 7.60 (s, 1H), 7.61 (t, 1H, J=2.0 Hz), 8.17-8.20 (m, 2H), 8.43 (s, 1H). LRMS: 422.7, 420.7 (M+1).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureAfter cooling to room temperature
  3. customthe reaction mixture was partitioned between dichloromethane (25 mL) and water (25 mL)
  4. dry with materialThe dichloromethane layer was dried over sodium sulfate (Na2SO4)
  5. concentrationconcentrated to dryness in vacuo