HRID518622

反应详情

EQUATION

反应方程式

HRID 518622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of (R)-tert-butyl 3-methyl-4-(cis-4-(5-nitro-2-(2-(piperidin-1-yl)ethoxy)pyridin-4-ylamino)cyclohexanecarbonyl)piperazine-1-carboxylate (0.2 g, 0.348 mmol) in MeOH (3.48 mL) was added tin(II) chloride (0.264 g, 1.392 mmol). The resulting suspension was stirred at 80° C. for 2 hours. The mixture was cooled to RT, diluted with EtOAc and washed with 1N aqueous NaOH. The organic layer was collected, dried over sodium sulfate and concentrated to afford (R)-tert-butyl 4-(cis-4-(5-amino-2-(2-(piperidin-1-yl)ethoxy)pyridin-4-ylamino)cyclohexanecarbonyl)-3-methylpiperazine-1-carboxylate as a tan solid (190 mg, 100%). MS m/z=545.4 [M+H]. Calc'd for C29H48N6O4: 544.4.

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. washwashed with 1N aqueous NaOH
  3. customThe organic layer was collected
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated