HRID1666506

反应详情

EQUATION

反应方程式

HRID 1666506 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl 4-(3-(5-(azetidin-1-yl)pyridin-2-yloxy)benzylidene)piperidine-1-carboxylate (0.135 g, 0.32 mmol) in CH2Cl2 (5 mL) cooled to 0° C. under a N2 atmosphere was added TFA (0.24 mL, 3.2 mmol). The resulting mixture was stirred for 1 h at RT. The solution was concentrated and then quenched with saturated NaHCO3 solution. The mixture was extracted with CH2Cl2. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to give the title compound (0.98 g, 96%). 1H NMR (500 MHz, DMSO-d6): δ 7.46 (s, 1H), 7.28 (s, 1H), 6.91 (d, J=7.5 Hz, 1H), 6.85 (m, 4H), 6.28 (s, 1H), 3.87 (t, J=7 Hz, 4H), 3.02 (m, 2H), 2.90 (m, 2H), 2.53 (m, 2H), 2.39 (m, 4H).

WORKUP

后处理

  1. concentrationThe solution was concentrated
  2. customquenched with saturated NaHCO3 solution
  3. extractionThe mixture was extracted with CH2Cl2
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated under reduced pressure