HRID273046

反应详情

EQUATION

反应方程式

HRID 273046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of (3-Nitro-pyridin-4-yl)-{4-[4-(3-pyrrolidin-1-yl-propoxy)-phenyl]-tetrahydro-pyran-4-ylmethyl}-amine (200 mg, 0.45 mmol) in ethanol (˜5 mL) was hydrogenated for 4 hours at room temperature at 40 psi in the presence of 10% Pd/C (20 mg, 10% w/w). The reaction mixture was filtered over Arbocel® and rinsed with ethanol. The filtrate was concentrated in vacuo to give a brown oily residue. The crude product was purified by flash chromatography on silica gel eluting with dichloromethane:methanol:ammonia (94:6:0.6, by volume) to provide the title compound (68 mg, 36%). HRMS ESI+ m/z 411.2750 [MH]+.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over Arbocel®
  2. washrinsed with ethanol
  3. concentrationThe filtrate was concentrated in vacuo
  4. customto give a brown oily residue
  5. customThe crude product was purified by flash chromatography on silica gel eluting with dichloromethane:methanol:ammonia (94:6:0.6, by volume)